APPLICATION ELEMENTS
`See MPEP chapter 600 concerning utility patent application contents.
`
`2.(cid:143)
`
`3.[x]
`
`1. [x] Fee Transmittal Form (e.g., PTO/SB/17)
`(Submit an original and a duplicate for fee processing)
`Applicant claims small entity status.
`See 37 CFR 1.27.
`[Total Pages
`Specification
`(preferred arrangement set forth below)
`- Descriptive title of the invention
`- Cross Reference to Related Applications
`- Statement Regarding Fed sponsored R & D
`• Reference to sequence listing, a table,
`or a computer program listing appendix
`- Background of the Invention
`• Brief"Summary of the·lnvention
`Brief Description of the Drawings (if filed)
`- Detailed Description
`• Claim(s)
`• Abstract of the Disclosure
`
`19
`
`•
`·l
`
`l
`
`.
`
`4.[x]
`
`Drawing(s) (35 U.S.C. 113)
`
`[Total Sheets
`
`1
`
`[Total Sheets
`5. Oath or Declaration
`a.O Newly executed (original or copy)
`b. [xj Copy from a prior application (37 CFR 1.63(d))
`(for continuation/divisional with Box 18 completed)
`
`3
`
`l
`
`I
`
`LO DELETION OF INVENTOB(Sl
`Signed statement attached deleting inventor(s)
`name in the prior application, see 37 CFR
`1.63(d)(2) and 1.33(b).
`
`6.0 Application Data Sheet. See 37 CFR 1.76
`
`(cid:143)
`
`Divisional
`
`Statements verifying identity of above copies
`ACCOMPANYING APPLICATION PARTS
`
`11.
`12. [x]
`
`9. (cid:143)
`10. (cid:143)
`(cid:143)
`(cid:143)
`(cid:143)
`(cid:143)
`17. (cid:143)
`
`15.
`
`16.
`
`Assignment Papers (cover sheet & document(s))
`37 CFR 3.73(b) Statement D Powerof
`(when there is an assignee)
`Attorney
`English Translation Document (iOlicable)
`Information Disclosure
`Copies of IDS
`Statement (IDS)/PT0-1449
`Citations
`13.
`Preliminary Amendment
`14. [x] Return Receipt Postcard (MPEP 503)
`(Should be specifically itemized)
`Certified Copy of Priority Document(s)
`(if foreign priority is claimed)
`Nonpublication Request under 35 U.S.C. 122
`(b)(2)(B)(i). Applicant must attach form PTO/SB/35
`or its equivalent.
`···········································································
`Other:
`..............................................................................
`18. If a CONTINUING APPLICATION, check appropriate box, and supply the requisite information below and in the first sentence of the
`specification following the title, or in an Application Data Sheet under 37 CFR 1. 76:
`D Continuation-in-part (CIP)
`Ix] Continuation
`of prior application No.: .J.QOJ~i~~-~---·······
`1732
`Mark2 Eashoo
`Art Unit:
`Examiner
`Prior application infonnation:
`For CONTINUATION OF DIVISIONAL APPS only; The entire disclosure of the prior application, from which an oath or declaration Is supplied under Box
`Sb, Is considered a part of the disclosure of the accompanying continuation or dlvlslonal application and Is hereby Incorporated by reference.
`The Incorporation can onlv be relied upon when a portion has been Inadvertently omitted from the submitted application parts.
`19. CORRESPONDENCE ADDRESS
`
`PTO/SB/05 (04-04)
`Approved for use through 07/31/2006. 0MB 0651-0032
`U.S. Patent and Trademark Office. U.S. DEPARTMENT OF COMMERCE
`Under the Paperwork Reduction Act of 1995, no persons are reQuired to respond to a collection of information unless it displays a valid 0MB control number.
`"I
`
`UTILITY
`PATENT APPLICATION
`TRANSMITTAL
`
`Attorney Docket No.
`
`Jadhav AC Cont
`
`First Inventor
`
`Prakash Mahadeo JADHA V
`
`Title
`
`See 1 in Addendum
`
`(Only for new nonprovisional applications under 37 CFR 1.53(b))
`
`Express Mail Label No.
`
`r-
`·u:,
`~
`
`\.
`
`ADDRESS TO:
`
`Commissioner for Patents
`P.O. Box 1450
`Alexandria VA 22313-1450
`
`1.(cid:143)
`
`CD-ROM or CD-R in duplicate, large table or
`Computer Program (Appendix)
`8. Nucleotide and/or Amino Acid Sequence Submission
`
`,)
`
`I
`
`I -
`' .
`I r"cr)
`0.:c:o
`Cl) C\J
`....,:,-..
`-
`(!)
`C':>0
`c.o-
`°'-r-
`~-r-
`..-
`
`(if a0 able, all necessary)
`(cid:143)
`(cid:143)
`
`Computer Readable Form (CRF)
`
`Specification Sequence Listing on:
`
`CD-ROM or CD-R (2 copies); or
`
`Paper
`
`i.
`
`ii.
`
`a.
`
`b.
`
`c.
`
`-(cid:143)
`
`W Customer Number: I
`
`23294
`
`I
`
`OR
`
`(cid:143)
`
`Correspondence address below
`
`Name
`
`Address
`City
`Country
`
`I State I
`I Telephone I
`Registration No. (Attorney/Agent) 47 003
`Date
`
`Zip Code
`Fax
`
`Name (PrinVType)
`Signature
`
`JenDifer P. Yancv
`.y'. VI} .,/A ,llu
`,· ;_
`'<.I;.,, ..
`I 02/18/2005
`This collection of informXi°" is requ\~/ 37 CFR 1.~(b). The inr6lmation is required to obtain or retain a benefit by the public which is to file (and by the
`USPTO to process) an
`plication. C nfidentiality is governed by 35 U.S.C. 122 and 37 CFR 1.14. This collection is estimated to take 12 minutes to complete,
`including gathering, preparing, and submitting the completed application form to the USPTO. Time will vary depending upon the individual case. Any comments on
`the amount of time you require to complete this form and/or suggestions for reducing this burden should be sent to the Chief Information Officer, U.S. Patent and
`Trademark Office, U.S. Department of Commerce, P.O. Box 1450, Alexandria, VA 22313-1450. DO NOT SEND FEES OR COMPLETED FORMS TO THIS
`ADDRESS. SEND TO: Commissioner for Patents, P.O. Box 1450, Alexandria, VA 22313-1450.
`If you need assistance in completing the fonn, call 1-800-PTO-9199 and select option 2.
`
`1
`
`TIDE 1002
`
`

`

`...
`
`,\
`
`Addendum
`
`1. A Process for Preparation of Chemically Stable, Dry-Flow, Low Compact, Dust Free,
`Soluble Granules of Phosphoroamidothioates
`
`2
`
`

`

`Effective on 12/08/2004.
`~ s oursuant to the Consolidated Approoriations Act. 2005 (H.R. 4818).
`
`PTO/SB/17 (12-04)
`Approved for use through 07/31/2006. 0MB 0651-0032
`U.S. Patent and Trademark Office; U.S. DEPARTMENT OF COMMERCE
`...
`..
`llnr1Rr lhR P::mRrwnrk RRri11r1inn A~I nf 1AA~ nn nA!l'lnns ::lrR r..n11irnrl In rA.snnnrl In ::1 mll~linn nf infnrm::itlnn 1inlAl'l.s it rli!'.nl::ivs ::1 v::ilirl OMR r.nntml n11mhRr
`Complete if Known
`
`Application Number
`
`Februarv 18 2005
`First Named Inventor Prakash Mahadeo JADHA V
`Eashoo, Mark
`Examiner Name
`1732
`Jadhav Ac Cont
`
`Attorney Docket No.
`
`Art Unit
`
`~
`
`..)
`
`r-en
`d FEE TRANSMITTAL Filing Date
`For FY 2005
`D Applicant claims small entity status. See 37 CFR 1.27
`\..TOTAL AMOUNT OF PAYMENT I ($)
`1,000.00
`CK] Check D Credit Card D Money Order (cid:143)
`
`METHOD OF PAYMENT (check all that aoolv)
`
`~ Deposit Account Deposit Account Number:
`
`None (cid:143)
`
`other (please identify):
`
`Deposit Account Name:
`
`10-1213
`Jennifer P. Yancy
`For the above-identified deposit account, the Director is hereby authorized to: (check all that apply)
`
`D Charge fee(s) indicated below, except for the filing fee
`[xJ Credit any overpayments
`
`charge fee(s) indicated below
`
`[Kl Charge any additional fee(s) or underpayments of fee(s)
`under 37 CFR 1.16 and 1.17
`WARNING: Information on this form may become publlc. Credit card information should not be Included on this form. Provide credit card
`Information and authorization on PTO-2038.
`FEE CALCULATION
`1. BASIC FILING, SEARCH, AND EXAMINATION FEES
`FILING FEES
`SEARCH FEES
`Small Enti~
`Small Enti~
`&ill} &ill}
`Fee($)
`300
`150
`250
`200
`100
`50
`200
`100
`150
`300
`150
`250
`200
`100
`0
`
`AgQlication Tirne
`Utility
`Design
`Plant
`Reissue
`Provisional
`2. EXCESS CLAIM FEES
`Small Enti~
`&ill}
`&ill}
`Fee Descritition
`50
`25
`Each claim over 20 or, for Reissues, each claim over 20 and more than in the original patent
`Each independent claim over 3 or, for Reissues, each independent claim more than in the original patent 200
`100
`180
`360
`Multiple dependent claims
`Total Claims
`Extra Claims
`15
`0
`- 20 or HP=
`X
`HP = highest number of total claims paid for, if greater than 20
`lndeg. Claims
`&ill}
`Extra Claim§
`0
`1
`=
`• 3 or HP =
`X
`HP = highest number of independent claims paid for, if greater than 3
`3. APPLICATION SIZE FEE
`If the specification and drawings exceed 100 sheets of paper, the application size fee due is $250 ($125 for small entity)
`for each additional 50 sheets or fraction thereof. See 35 U.S.C. 4l(a)(l)(G) and 37 CFR 1.16(s).
`Number of each additional 50 or fra,tion thereof &ill}
`Total Sheets
`Extra Sh1:11:111i
`-80
`20
`250.00
`- 100 =
`(round up to a whole number) X
`4. OTHER FEE(S)
`Non-English Specification, $130 fee (no small entity discount)
`Other:
`
`&ill}
`500
`100
`300
`500
`0
`
`Fees Paid {il
`1,000.00
`
`EXAMINATION FEES
`Small Enti~
`Fee($)
`100
`65
`80
`300
`0
`
`&ill}
`200
`130
`160
`600
`0
`
`il
`
`1(
`
`Fee Paid Ii)
`Multi12le De12endent Claims
`0 00 ~ Fee Paid
`
`=
`
`llilfil
`
`Fee Paid (il
`0 00
`
`150 =
`
`=
`
`Fee Paid {il
`Q QQ
`Fees Paid (il
`
`SUBMITTED BY
`
`Signature
`
`A
`
`I Registration No.
`
`CAttomev/Aaenll
`
`(I
`
`47,003
`
`Telephone
`
`Date
`
`-ef JJ A A
`I ' / { , :P. iln !" ~., _
`703-4151-500
`I
`Februarv 18. 2005
`Name (Print/Type) {ennifer P. tS!'ancv
`This collection of information is required by 37 CFR 1.136. The information is required to obtain or retain a benefit by the public which is to file (and by the
`USPTO to process) an application. Confidentiality is governed by 35 U.S.C. 122 and 37 CFR 1.14. This collection is estimated to take 30 minutes to complete,
`including gathering, preparing, and submitting the completed application form to the USPTO. Time will vary depending upon the individual case. Any comments
`on the amount of time you require to complete this form and/or suggestions for reducing this burden, should be sent to the Chief Information Officer, U.S. Patent
`and Trademark Office, U.S. Department of Commerce, P.O. Box 1450, Alexandria, VA 22313-1450. DO NOT SEND FEES OR COMPLETED FORMS TO THIS
`ADDRESS. SEND TO: Commissioner for Patents, P.O. Box 1450, Alexandria, VA 22313-1450.
`If you need assistance in completing the form, ca/11-800-PTO-9199 and select option 2.
`
`3
`
`(cid:143)
`

`

`APPLICATION ELEMENTS
`See MPEP chapter 600 concerning utility patent application contents.
`
`2.(cid:143)
`
`3.[x]
`
`1. [x] Fee Transmittal Form (e.g., PTO/SB/17)
`(Submit an original and a duplicate for fee processing)
`Applicant claims small entity status.
`See 37 CFR 1.27.
`[Total Pages
`Specification
`(preferred arrangement set forth below)
`- Descriptive title of the invention
`- Cross Reference to Related Applications
`- Statement Regarding Fed sponsored R & D
`• Reference to sequence listing, a table,
`or a computer program listing appendix
`- Background of the Invention
`• Brief"Summary of the·lnvention
`Brief Description of the Drawings (if filed)
`- Detailed Description
`• Claim(s)
`• Abstract of the Disclosure
`
`19
`
`•
`·l
`
`l
`
`.
`
`4.[x]
`
`Drawing(s) (35 U.S.C. 113)
`
`[Total Sheets
`
`1
`
`[Total Sheets
`5. Oath or Declaration
`a.O Newly executed (original or copy)
`b. [xj Copy from a prior application (37 CFR 1.63(d))
`(for continuation/divisional with Box 18 completed)
`
`3
`
`l
`
`I
`
`LO DELETION OF INVENTOB(Sl
`Signed statement attached deleting inventor(s)
`name in the prior application, see 37 CFR
`1.63(d)(2) and 1.33(b).
`
`6.0 Application Data Sheet. See 37 CFR 1.76
`
`(cid:143)
`
`Divisional
`
`Statements verifying identity of above copies
`ACCOMPANYING APPLICATION PARTS
`
`11.
`12. [x]
`
`9. (cid:143)
`10. (cid:143)
`(cid:143)
`(cid:143)
`(cid:143)
`(cid:143)
`17. (cid:143)
`
`15.
`
`16.
`
`Assignment Papers (cover sheet & document(s))
`37 CFR 3.73(b) Statement D Powerof
`(when there is an assignee)
`Attorney
`English Translation Document (iOlicable)
`Information Disclosure
`Copies of IDS
`Statement (IDS)/PT0-1449
`Citations
`13.
`Preliminary Amendment
`14. [x] Return Receipt Postcard (MPEP 503)
`(Should be specifically itemized)
`Certified Copy of Priority Document(s)
`(if foreign priority is claimed)
`Nonpublication Request under 35 U.S.C. 122
`(b)(2)(B)(i). Applicant must attach form PTO/SB/35
`or its equivalent.
`···········································································
`Other:
`..............................................................................
`18. If a CONTINUING APPLICATION, check appropriate box, and supply the requisite information below and in the first sentence of the
`specification following the title, or in an Application Data Sheet under 37 CFR 1. 76:
`D Continuation-in-part (CIP)
`Ix] Continuation
`of prior application No.: .J.QOJ~i~~-~---·······
`1732
`Mark2 Eashoo
`Art Unit:
`Examiner
`Prior application infonnation:
`For CONTINUATION OF DIVISIONAL APPS only; The entire disclosure of the prior application, from which an oath or declaration Is supplied under Box
`Sb, Is considered a part of the disclosure of the accompanying continuation or dlvlslonal application and Is hereby Incorporated by reference.
`The Incorporation can onlv be relied upon when a portion has been Inadvertently omitted from the submitted application parts.
`19. CORRESPONDENCE ADDRESS
`
`PTO/SB/05 (04-04)
`Approved for use through 07/31/2006. 0MB 0651-0032
`U.S. Patent and Trademark Office. U.S. DEPARTMENT OF COMMERCE
`Under the Paperwork Reduction Act of 1995, no persons are reQuired to respond to a collection of information unless it displays a valid 0MB control number.
`"I
`
`UTILITY
`PATENT APPLICATION
`TRANSMITTAL
`
`Attorney Docket No.
`
`Jadhav AC Cont
`
`First Inventor
`
`Prakash Mahadeo JADHA V
`
`Title
`
`See 1 in Addendum
`
`(Only for new nonprovisional applications under 37 CFR 1.53(b))
`
`Express Mail Label No.
`
`r-
`·u:,
`~
`
`\.
`
`ADDRESS TO:
`
`Commissioner for Patents
`P.O. Box 1450
`Alexandria VA 22313-1450
`
`1.(cid:143)
`
`CD-ROM or CD-R in duplicate, large table or
`Computer Program (Appendix)
`8. Nucleotide and/or Amino Acid Sequence Submission
`
`,)
`
`I
`
`I -
`' .
`I r"cr)
`0.:c:o
`Cl) C\J
`....,:,-..
`-
`(!)
`C':>0
`c.o-
`°'-r-
`~-r-
`..-
`
`(if a0 able, all necessary)
`(cid:143)
`(cid:143)
`
`Computer Readable Form (CRF)
`
`Specification Sequence Listing on:
`
`CD-ROM or CD-R (2 copies); or
`
`Paper
`
`i.
`
`ii.
`
`a.
`
`b.
`
`c.
`
`-(cid:143)
`
`W Customer Number: I
`
`23294
`
`I
`
`OR
`
`(cid:143)
`
`Correspondence address below
`
`Name
`
`Address
`City
`Country
`
`I State I
`I Telephone I
`Registration No. (Attorney/Agent) 47 003
`Date
`
`Zip Code
`Fax
`
`Name (PrinVType)
`Signature
`
`JenDifer P. Yancv
`.y'. VI} .,/A ,llu
`,· ;_
`'<.I;.,, ..
`I 02/18/2005
`This collection of informXi°" is requ\~/ 37 CFR 1.~(b). The inr6lmation is required to obtain or retain a benefit by the public which is to file (and by the
`USPTO to process) an
`plication. C nfidentiality is governed by 35 U.S.C. 122 and 37 CFR 1.14. This collection is estimated to take 12 minutes to complete,
`including gathering, preparing, and submitting the completed application form to the USPTO. Time will vary depending upon the individual case. Any comments on
`the amount of time you require to complete this form and/or suggestions for reducing this burden should be sent to the Chief Information Officer, U.S. Patent and
`Trademark Office, U.S. Department of Commerce, P.O. Box 1450, Alexandria, VA 22313-1450. DO NOT SEND FEES OR COMPLETED FORMS TO THIS
`ADDRESS. SEND TO: Commissioner for Patents, P.O. Box 1450, Alexandria, VA 22313-1450.
`If you need assistance in completing the fonn, call 1-800-PTO-9199 and select option 2.
`
`4
`
`

`

`...
`
`,\
`
`Addendum
`
`1. A Process for Preparation of Chemically Stable, Dry-Flow, Low Compact, Dust Free,
`Soluble Granules of Phosphoroamidothioates
`
`5
`
`

`

`Effective on 12/08/2004.
`~ s oursuant to the Consolidated Approoriations Act. 2005 (H.R. 4818).
`
`PTO/SB/17 (12-04)
`Approved for use through 07/31/2006. 0MB 0651-0032
`U.S. Patent and Trademark Office; U.S. DEPARTMENT OF COMMERCE
`...
`..
`llnr1Rr lhR P::mRrwnrk RRri11r1inn A~I nf 1AA~ nn nA!l'lnns ::lrR r..n11irnrl In rA.snnnrl In ::1 mll~linn nf infnrm::itlnn 1inlAl'l.s it rli!'.nl::ivs ::1 v::ilirl OMR r.nntml n11mhRr
`Complete if Known
`
`Application Number
`
`Februarv 18 2005
`First Named Inventor Prakash Mahadeo JADHA V
`Eashoo, Mark
`Examiner Name
`1732
`Jadhav Ac Cont
`
`Attorney Docket No.
`
`Art Unit
`
`~
`
`..)
`
`r-en
`d FEE TRANSMITTAL Filing Date
`For FY 2005
`D Applicant claims small entity status. See 37 CFR 1.27
`\..TOTAL AMOUNT OF PAYMENT I ($)
`1,000.00
`CK] Check D Credit Card D Money Order (cid:143)
`
`METHOD OF PAYMENT (check all that aoolv)
`
`~ Deposit Account Deposit Account Number:
`
`None (cid:143)
`
`other (please identify):
`
`Deposit Account Name:
`
`10-1213
`Jennifer P. Yancy
`For the above-identified deposit account, the Director is hereby authorized to: (check all that apply)
`
`D Charge fee(s) indicated below, except for the filing fee
`[xJ Credit any overpayments
`
`charge fee(s) indicated below
`
`[Kl Charge any additional fee(s) or underpayments of fee(s)
`under 37 CFR 1.16 and 1.17
`WARNING: Information on this form may become publlc. Credit card information should not be Included on this form. Provide credit card
`Information and authorization on PTO-2038.
`FEE CALCULATION
`1. BASIC FILING, SEARCH, AND EXAMINATION FEES
`FILING FEES
`SEARCH FEES
`Small Enti~
`Small Enti~
`&ill} &ill}
`Fee($)
`300
`150
`250
`200
`100
`50
`200
`100
`150
`300
`150
`250
`200
`100
`0
`
`AgQlication Tirne
`Utility
`Design
`Plant
`Reissue
`Provisional
`2. EXCESS CLAIM FEES
`Small Enti~
`&ill}
`&ill}
`Fee Descritition
`50
`25
`Each claim over 20 or, for Reissues, each claim over 20 and more than in the original patent
`Each independent claim over 3 or, for Reissues, each independent claim more than in the original patent 200
`100
`180
`360
`Multiple dependent claims
`Total Claims
`Extra Claims
`15
`0
`- 20 or HP=
`X
`HP = highest number of total claims paid for, if greater than 20
`lndeg. Claims
`&ill}
`Extra Claim§
`0
`1
`=
`• 3 or HP =
`X
`HP = highest number of independent claims paid for, if greater than 3
`3. APPLICATION SIZE FEE
`If the specification and drawings exceed 100 sheets of paper, the application size fee due is $250 ($125 for small entity)
`for each additional 50 sheets or fraction thereof. See 35 U.S.C. 4l(a)(l)(G) and 37 CFR 1.16(s).
`Number of each additional 50 or fra,tion thereof &ill}
`Total Sheets
`Extra Sh1:11:111i
`-80
`20
`250.00
`- 100 =
`(round up to a whole number) X
`4. OTHER FEE(S)
`Non-English Specification, $130 fee (no small entity discount)
`Other:
`
`&ill}
`500
`100
`300
`500
`0
`
`Fees Paid {il
`1,000.00
`
`EXAMINATION FEES
`Small Enti~
`Fee($)
`100
`65
`80
`300
`0
`
`&ill}
`200
`130
`160
`600
`0
`
`il
`
`1(
`
`Fee Paid Ii)
`Multi12le De12endent Claims
`0 00 ~ Fee Paid
`
`=
`
`llilfil
`
`Fee Paid (il
`0 00
`
`150 =
`
`=
`
`Fee Paid {il
`Q QQ
`Fees Paid (il
`
`SUBMITTED BY
`
`Signature
`
`A
`
`I Registration No.
`
`CAttomev/Aaenll
`
`(I
`
`47,003
`
`Telephone
`
`Date
`
`-ef JJ A A
`I ' / { , :P. iln !" ~., _
`703-4151-500
`I
`Februarv 18. 2005
`Name (Print/Type) {ennifer P. tS!'ancv
`This collection of information is required by 37 CFR 1.136. The information is required to obtain or retain a benefit by the public which is to file (and by the
`USPTO to process) an application. Confidentiality is governed by 35 U.S.C. 122 and 37 CFR 1.14. This collection is estimated to take 30 minutes to complete,
`including gathering, preparing, and submitting the completed application form to the USPTO. Time will vary depending upon the individual case. Any comments
`on the amount of time you require to complete this form and/or suggestions for reducing this burden, should be sent to the Chief Information Officer, U.S. Patent
`and Trademark Office, U.S. Department of Commerce, P.O. Box 1450, Alexandria, VA 22313-1450. DO NOT SEND FEES OR COMPLETED FORMS TO THIS
`ADDRESS. SEND TO: Commissioner for Patents, P.O. Box 1450, Alexandria, VA 22313-1450.
`If you need assistance in completing the form, ca/11-800-PTO-9199 and select option 2.
`
`6
`
`(cid:143)
`

`

`A PROCESS FOR PREPARATION OF CHEMICALLY STABLE, DRY~FLOW, LOW
`
`COMPACT, DUST FREE, SOLUBLE GRANULES OF PHOSPHOROAMIDOTHIOATES
`
`CROSS REFERENCE TO RELATED APPLICATION
`
`5
`
`[0001] This application claims the benefit, under 35 U.S.C. 119(e), of U.S. Provisional
`
`Application No. 60/340,272 filed December 18, 2001, the contents of which are incorporated
`
`herein by reference.
`
`[0002] This application is a continuation application of U.S. Serial No. 10/126,965 filed April
`
`22, 2002, the contents of which are incorporated herein by reference.
`
`10
`
`1. Field of the Invention
`
`BACKGROUND OF THE INVENTION
`
`[0003] The present invention relates to a process for preparing insecticidally active soluble
`
`granules of phosphoroamidothioate, referred to herein as acephate.
`
`15
`
`2. Background Information
`
`[0004] In recent years, agricultural chemicals have been most preferably formulated in the
`
`form of dusts, wettable powders, soluble powders, emulsifiable concentrates, soluble liquid/
`
`concentrates, granules, coated granules, water dispersible granules, suspension concentrates,
`
`and solutions. Occasionally, when dusts are produced by absorbing or mixing active
`
`20
`
`ingredients with a finely divided inert carrier material, for example China Clay or the like, drift
`
`problems occur. With wettable powders and soluble powders the problems faced at the time of
`
`dilution are not only drift, but the final disposal of containers, for dust particles tend to stick to
`
`7
`
`

`

`sides of the containers. The left over materials within the containers pose great problems to
`
`the environment, operators and users.
`
`[0005] Although dusts are undesirable because of airborne contamination and handling
`
`difficulties, liquid spray formulations have not provided an acceptable alternative, for they
`
`5
`
`involve solvents and packaging expenses, along with container disposal requirements that
`
`detract from their commercial desirability.
`
`[0006] Water dispersible granules produced by fluidized bed spray dryers overcome the
`
`problems associated with wettable powders and soluble powders, but have high processing
`
`costs and require high value capital investment, as well as requiring highly skilled staff. These
`
`Io
`
`problems impose a significant barrier in widening the market acceptance of these compounds.
`
`[0007] Certain phosphoroamidothioates and phosphoroamidodithioates, collectively referred
`
`to as Phosphoroamidothioates, are known to have excellent insecticidal activity against a
`
`variety of insects and in a variety of environments. Acephate, one of the important commercial
`
`insecticides within this class of compounds, is a systemic and contact insecticide of moderate
`
`15
`
`persistence with residual activity lasting about 10-15 days. It is effective against a wide range
`
`of aphids, leaf-miners, lepidopterous, larvae, sawflies and thrips and it is also a non-phytotoxic
`
`on many crop plants.
`
`[0008] Phosphoroamidothioate containing pellets have been proposed in the past, but
`
`difficulties have been encountered in pelletizing acephate technical, the preferred insecticide
`
`20 within the class of phosphoroamidothioates. Attempts to manufacture acephate technical
`
`pellets from acephate technical powders have been proposed and have been unsuccessful.
`
`[0009] Considerable experimentation in the area of producing the preferred high-strength
`
`acephate granules has been conducted and confirms the manufacturing difficulties which
`
`2
`
`8
`
`

`

`earlier formulators have experienced. Furthermore, the pellets and methods proposed for
`
`making pellets suggested in the prior art leave considerable room for improvement. Prior
`
`extrusion processes have proposed the addition of costly surfactants, the combination of
`
`phosphoroamidothioate with a second active ingredient, or the creation of a mixture of the
`
`5
`
`active ingredient with a solvent in an amount of from 3-25% by weight before extrusion, but
`
`these processes have not solved the problems encountered.
`
`[0010] The formulation of acephate presently in use is acephate 75% soluble powder having
`
`acephate active ingredient 75% (w/w), surfactant 1 to 2% (w/w), inert filler (precipitated silica)
`
`to make 100% (w/w). Acephate 75% soluble powder poses the problems of dust, low
`
`10
`
`pourability, high transportation costs, high capital manufacturing investment, measurement
`
`difficulties, difficulties in packing material disposal, handling problems, high risk of caking
`
`and others.
`
`[0011] Because of
`
`the problems associated with producing granular
`
`forms of
`
`phosphoroamidothioates, such as the preferred acephate, there is a need in the art for a process
`
`15
`
`for preparing chemically stable, dry flow, low compact, dust free, insecticidally active soluble
`
`granules of phosphoroamidothioate which are useful from a practical stand point, as well as for
`
`a low cost, practical manufacturing technique which can be practiced on a commercial scale
`
`without requiring expensive additives or solvents.
`
`20
`
`SUMMARY OF THE INVENTION.
`
`[0012] By the present invention the above-identified major limitations have been overcome.
`
`The method for producing dry flow, low-compact, dust free, soluble phosphoroamidothioate
`
`granules, such as
`
`the preferred compound acephate,
`
`is an
`
`improvement over prior
`
`3
`
`9
`
`

`

`manufacturing processes. Further, the dust free soluble granules produced by this invention,
`
`which has a concentration of the insecticidally active ingredient in this formulation may vary
`
`from 40-98% of phosphoroamidothioate active ingredient, is more advantageous than prior
`
`granular products and exhibits certain very desirable characteristics as noted hereinafter.
`
`5
`
`[0013] Briefly, and in accordance with a preferred embodiment of the invention, dry flow, low
`
`compact, dust free, soluble granules of insecticially active phosphoroamidothioate are prepared
`
`by forming a pre-mix containing the required quantity of phosphoroamidothioate, a dispersing
`
`agent, a wetting agent, a binding agent, an antifoaming agent, a disintegrating agent, a
`
`stabilizer and filler. The specified adjuvants have a maximum of 1 % water insoluble matter.
`
`Io
`
`This pre-mix is then ground to produce a ground product having preferred particle sizes
`
`between 5.0 microns to 10.0 microns. The ground product is fed to a post-mixer to form a
`
`mixture. The mixture is then fed through a hopper into a granulator where granules are
`
`formed. The granules are then dried, and the dried granules are sized and sieved to separate
`
`dry granules from fines, producing dry flow, low compact, dust free, soluble granules of
`
`15
`
`phosphoro-amidothioate as noted above, the preferred phosphoroamidothioate is acephate.
`
`The fines may be recycled back to the post mixer.
`
`[0014) This invention produces essentially dry flow,
`
`low compact, dust free soluble
`
`phosphoroamidothioate granules having a preferred granule size of 1.5 to 3.0 mm in length and
`
`0.5 to 1.0 mm in diameter. These granules of phosphoroamidothioates are characterized by
`
`20
`
`aging stability for a minimum of two years.
`
`4
`
`10
`
`

`

`BRIEF DESCRIPTION OF THE DRAWINGS
`
`[0015) The features and advantages of the present invention will become apparent from the
`
`following detailed description of preferred embodiments thereof, taken in conjunction with the
`
`accompanying drawings, in which:
`
`5
`
`FIG. 1 is a flow chart of the preferred embodiment of the present invention.
`
`DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
`
`[0016) The process of the present invention is best described by referring to the flow chart in
`
`FIG. 1. An essentially dry pre-mix comprising about 95% to 99% of solids and 1 % to 5%
`
`10 moisture and/or solvent is formed from the following ingredients: 40% to 98% of the
`
`insecticidally active compound 2, 0.1% to 5.0% dispersing agent 4, 0.1% to 3.0% wetting
`
`agent 6, 0.1 % to 3 .0% binding agent 8, 0.01 % to 0.08% antifoaming agent 10, 0.01 % to 10,0%
`
`disintegrating agent 12, 0.01 % to 1.0% stabilizer 14, and fillers 16 to make 100% (w/w). The
`
`insecticidally active compounds of the present invention have the following formula:
`
`15
`
`0
`II
`o
`C -. -R2
`R- y '------ ~
`P -N /
`R,-s/
`\
`
`R3
`
`wherein R and R 1 individually are an alkyl, alkenyl or alkynyl group containing up to 6
`
`carbon atoms, R 2 is hydrogen, an alkyl group containing 1 to 18 carbon atoms, a cycloalkyl
`
`group containing 3 to 8 carbon atoms, an alkenyl group containins 2 to 18 carbon atoms or an
`
`5
`
`11
`
`

`

`alkynyl group containing 3 to 18 carbon atoms, R 3 is hydrogen or an alkyl group containing 1
`
`to 6 carbon atoms, and Y is oxygen or sulfur. All of the inert ingredients are preferably solids
`
`and in a powder form.
`
`In one preferred embodiment, the binding agent 8 is selected from
`
`sucrose and starch derivatives or a blend thereof, the wetting agent 6 is selected from calcium
`
`5
`
`or sodium salt of alkyl aryl sulphonate, the dispersing agent 4 is selected from the derivative of
`
`sulfonated fatty alcohols, the disintegrating agent 12 is selected from swelling type clays such
`
`as Bentonite and zeolite, the antifoaming agent 10 is selected from silicon oil derivatives, the
`
`stabiliser 14 is selected from salts of higher fatty acids, and the filler 16 is selected from
`
`precipitated silica and kaoline and the like. Grinding 22 of the pre-mix 20 is then conducted,
`
`10
`
`preferably in a microniser, to obtain a ground product 24 having a preferred particle size of 5
`
`microns to 10 microns.
`
`[0017] The ground product 24 is subjected to post-mixing 26 to form a mixture 28 which is
`
`then made into granules 36 by preferably charging 30, by way of a rotary feeder, a feeding
`
`hopper which supplies the mixture to a granulator for granulation 34. The granulator that
`
`15
`
`performs the granulation 34 has a preferred inlet temperature between 30 to 35°C and a
`
`preferred outlet temperature of between 40°C to 45°C. The resulting granules 36 are subjected
`
`to a drying 38 process, preferably by passing the granules 36 through an air chamber,
`
`producing dry granules 40.
`
`[0018] Sizing 42 the dry granules 40 is then accomplished to produce sized granules 44 of a
`
`20
`
`desired length and diameter. Sizing the granules is preferably conducted by passing the dry
`
`granules 40 through an oscillating cutter to obtain granules which are preferably between about
`
`1.5 mm and 3.0 mm in length and 0.5 mm to 1.0 mm in diameter. After sizing, the sized
`
`6
`
`12
`
`

`

`granules 44 are subjected to sieving 46 to separate fines 50 generated during the sizing process
`
`from desired dust free soluble granules 51.
`
`[0019) The fines 50 from the sieving 46 process may be collected and recycled at the charging
`
`30 stage of the process to obtain a minimum yield of 99.0% dry :flowable, low compact, dust
`
`5
`
`free, soluble granules 54 of phosphoroamidothioates, preferably acephate.
`
`[0020) The dust free soluble granules 54 were tested for required quality specifications and
`
`packed in desired packing. This technique gives 99% of conversion yield. The dust free soluble
`
`granules 54 enjoy all the formulation advantages described above, producing dust free soluble
`
`granules 54 which are beneficial from an economic aspect and a handling aspect and which
`
`1 o
`
`show a very good performance during use.
`
`[0021) The following examples are presented to illustrate but not to restrict the present
`
`invention. Parts and percentage are by weight unless otherwise specified.
`
`[0022) Acephate 97% Granules can be prepared as follows:
`
`EXAMPLE 1
`
`15
`
`Composition
`
`Ingredients
`
`Quantity (% w/w)
`
`Acephate Technical 98.5% purity
`
`Dispersing agent
`
`Wetting agent
`
`20
`
`Binding agent
`
`Antifoaming agent
`
`Disintegrating agent
`
`Stabilizer
`
`98.48
`
`0.50
`
`0.10
`
`0.10
`
`0.03
`
`0.50
`
`0.05
`
`7
`
`13
`
`

`

`Filler
`
`0.24
`
`Total ...
`
`100.00
`
`EXAMPLE 1 PROCESS:
`
`5
`
`(0023) The constituents of the above composition are mixed in a pre-mixer, then ground in a
`
`microniser to the required size of 5 micron to 10 micron. The ground product 24 is again
`
`mixed in a post-mixer to get a uniform homogeneous mixture 28. This homogeneous mixture
`
`28 is then fed through a rotary feeder into a low compaction granulator, while maintaining an
`
`inlet temperature of 32 to 35°C and an outlet temperature of 40 to 45°C. The Acephate
`
`10
`
`granules 36.formed in the granulator are further dried through an air chamber, sized to 1.5 mm
`
`to 3 mm length, and are collected. The fines 50 generated during the process are recharged to
`
`get a conversion yield of 99 percent.
`
`[0024) Acephate 98% granules can be prepared as follows:
`
`EXAMPLE2
`
`15
`
`Composition
`
`Ingredient
`
`Quantity (% w/w)
`
`Acephate Technical 98.5% purity
`
`Dispersing agent
`
`Wetting agent
`
`20
`
`Binding agent
`
`Antifoaming agent
`
`Disintegrating agent
`
`Stabilizer
`
`99.50
`
`0.25
`
`0.03
`
`0.05
`
`0.02
`
`0.05
`
`0.05
`
`8
`
`14
`
`

`

`Filler
`
`Total
`
`0.05
`
`100.00
`
`[0025) Acephate 98% granules with above composition can be prepared by following the
`
`5
`
`process described in EXAMPLE 1.
`
`[0026) Acephate 97.5% granules can be prepared as follows:
`
`EXAMPLE