TRANSLATOR CERTIFICATION
`
`Date: June 2, 2020
`
`To whom it may concern:
`
`I, Samuel Chong, a translator fluent in the Chinese and English languages, on behalf of
`Morningside Translations, do solemnly and sincerely declare that the following is, to the best of
`my knowledge and belief, a true and correct translation of the documents listed below in a
`form that reflects the intention and meaning of the original text.
`
`I hereby declare that all statements made herein of my own knowledge are true and that all
`statements made on information and belief are believed to be true; and further that these
`statements were made with the knowledge that willful false statements and the like so made
`are punishable by fine or imprisonment, or both, under Section 1001 of Title 18 of the United
`States Code.
`
`The document is designated as:
`
`Chinese Patent CN 1127588 A
`
`Signature
`
`Samuel Chong
`
`Print
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`CERT-11, 2019-APR-12, V1
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`1
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`TIDE 1007
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`(19) PATENT OFFICE OF THE PEOPLE’S REPUBLIC OF CHINA
`[11] PUBLICATION NUMBER: CN 1127588A
`[12] INVENTION PATENT APPLICATION
`PUBLICATION
`[21] APPLICATION NUMBER: 94119540.6
`[51] Int. Cl6
`A01N 57 / 28
`[74] PATENT AGENCY: CCPIT PATENT
`AND TRADEMARK LAW OFFICE
`AGENT: JING QUAN
`A01N 25 / 12
`
`
`
`[43] PUBLICATION DATE: JULY 31, 1996
`
`[22] APPLICATION DATE: DECEMBER 20, 1994
`[30] PRIORITY
`[32] 93.12.20[33]JP[31]319595 / 93
`[32] 94.5.9 [33]JP[31]094813 / 94
`[71] APPLICANT: SUMITOMO CHEMICAL CO.,
`LTD.
`ADDRESS: OSAKA, JAPAN
`
`|72] INVENTOR: YAMADA MASAHIRO,
`KATAYAMA YASUYUKI OTSUBO TOSHIRO
`
`
`
`
`[54] Title of Invention
`Method for Stabilizing Acephate and Dry
`Pesticide Preparation Containing Stabilized
`Acephate
`[57] Abstract
`The present invention relates to a method for
`stabilizing acephate. The method comprises
`adding condensed sodium phosphate and/or
`synthetic silicic acid with alkylsilylated silanol
`groups on the surface to acephate or a dry
`pesticide preparation containing acephate, and
`relates to stabilized acephate added with
`condensed sodium phosphate and/or synthetic
`silicic acid with alkylsilylated silanol groups on
`the surface.
`
`
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`CLAIMS 1 PAGE DESCRIPTION 5 PAGES
`DRAWINGS 0 PAGES
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` (BJ) No. 1456
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`Claims
`
`What is claimed is:
`1. A method for stabilizing acephate, comprising adding an effective amount of
`condensed sodium phosphate and/or an effective amount of synthetic silicic acid
`with alkylsilylated silanol groups on the surface to acephate.
`2. A method for stabilizing acephate in a dry preparation, comprising mixing
`acephate with an effective amount of condensed sodium phosphate.
`3. A method according to claim 2, wherein a weight ratio between acephate and
`condensed sodium phosphate is 1: 0.01 to 1: 10.
`4. A method for stabilizing acephate in a dry preparation, comprising mixing
`acephate with an effective amount of synthetic silicic acid with alkylsilylated
`silanol groups on the surface.
`5. A method according to claim 4, wherein a weight ratio between acephate and
`synthetic silicic acid with alkylsilylated silanol groups on the surface is 1: 0.05 to
`1: 10.
`6. A dry pesticide preparation, comprising acephate and an effective amount of
`condensed sodium phosphate and/or an effective amount of synthetic silicic acid
`with alkylsilylated silanol groups on the surface.
`7. A dry pesticide preparation, comprising acephate and an effective amount of
`condensed sodium phosphate.
`8. A dry pesticide preparation, comprising acephate and an effective amount of
`synthetic silicic acid with alkylsilylated silanol groups on the surface.
`9. A dry pesticide preparation according to claim 7, wherein a weight ratio between
`acephate and condensed sodium phosphate is 1: 0.01 to 1: 10.
`10. A dry pesticide preparation according to claim 8, wherein a weight ratio between
`acephate and synthetic silicic acid with alkylsilylated silanol groups on the
`surface is 1: 0.05 to 1: 10.
`11. A dry pesticide preparation according to claim 7, wherein the preparation is
`dustable powder, non-floating dustable powder, wettable powder, water soluble
`powder, granule, water soluble granule, water dispersible granule, dry flowable,
`tablet or pill.
`12. A dry pesticide preparation according to claim 7, wherein the preparation is
`dustable powder, non-floating dustable powder, water soluble powder, granule,
`water soluble granule, water dispersible granule, dry flowable, tablet or pill.
`13. A dry pesticide preparation according to claim 8, wherein the preparation is
`dustable powder, non-floating dustable powder, wettable powder, water soluble
`powder, granule, water soluble granule, water dispersible granule, dry flowable,
`tablet or pill.
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`Description
`
`Method for Stabilizing Acephate and Dry Pesticide Preparation
`Containing Stabilized Acephate
`
`The present invention relates to a method for stabilizing acephate and a dry pesticide
`preparation containing stabilized acephate.
`Acephate (O,S-dimethyl-N-acetylthiophosphoramidate) is a known compound with
`insecticidal activity as described at the first page of the Pesticide Manual Edition 8
`(published by the British Crop Protection Cuncil, 1987), and currently is used as an
`active ingredient for agricultural insecticide because it has effective control activity
`against various pests and diseases.
`In contrast to other organophosphorus compounds with insecticidal activity, acephate
`is less stable in pesticide preparations. Therefore, acephate in the preparations may be
`decomposed violently with the change of storage conditions, thereby unable to
`effectively show activity all the time. Under these circumstances, there is a need for a
`method to impart stability to acephate in the preparations, and a need to develop a
`pesticide composition that can effectively play the insecticidal activity of acephate.
`The inventors conducted extensive research on this subject and found that condensed
`sodium phosphate and/or synthetic silicic acid with alkylsilylated silanol groups on
`the surface can improve the stability of acephate in dry preparations, thereby
`completing the present invention.
`Therefore, the present invention relates to a method for stabilizing acephate, i.e.,
`adding an effective amount of condensed sodium phosphate and/or an effective
`amount of synthetic silicic acid with alkylsilylated silanol groups on the surface to
`acephate; relates to a method for stabilizing acephate in a dry preparation, i.e., mixing
`acephate with an effective amount of condensed sodium phosphate and/or an effective
`amount of synthetic silicic acid with alkylsilylated silanol groups on the surface; and a
`dry pesticide preparation containing acephate and an effective amount of condensed
`sodium phosphate and/or an effective amount of synthetic silicic acid with
`alkylsilylated silanol groups on the surface.
`In the scope of the present invention, condensed sodium phosphate refers to a
`compound made by condensing two or more sodium phosphates via an oxygen atom,
`such as sodium polyphosphate, sodium tripolyphosphate or sodium pyrophosphate.
`The synthetic silicic acid with alkylsilylated silanol groups on the surface used in the
`present invention can generally be prepared by the following method: use dialkyl
`dichlorosilane or alkyl trichlorosilane to alkylsilyate wet-method synthetic silicic acid
`obtained by adding an inorganic acid (such as hydrochloric acid and sulfuric acid) to a
`sodium silicate water solution or dry-method synthetic silicic acid obtained by using
`oxyhydrogen flame to decompose silicon tetrachloride. The alkyl is generally a lower
`alkyl group, such as methyl and ethyl, and the number of silanol groups on the surface
`is generally significantly reduced to 3 or less/nm2. The synthetic silicic acid with
`alkylsilylated silanol groups on the surface obtained in this way are available on the
`market, such as Carples® CS-701 or Carplex® CS-801 produced by Shionogi
`Pharmaceuticals, Reolosil® MT-10 produced by Tokuyama Soda, and Aerosil® R972,
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`Sipernat® D17 or Sipernat® D10 produced by Degussa.
`The amount of condensed sodium phosphate for stabilizing acephate is generally 0.01
`to 10 parts by weight per part by weight of acephate, preferably 0.05 to 1 part by
`weight per part by weight of acephate.
`The amount of synthetic silicic acid with alkylsilylated silanol groups on the surface
`for stabilizing acephate is generally 0.05 part by weight or more per part by weight of
`acephate, preferably 0.05 to 10 parts by weight per part by weight of acephate.
`The content of acephate in a dry pesticide preparation described in the present
`invention is generally 0.5 to 99 (wt) %, preferably 5 to 95 (wt) %. The content of
`condensed sodium phosphate in the dry pesticide preparation is an amount that can
`stabilize acephate, generally 0.01 to 50 (wt) %, preferably 1 to 20 (wt) %, more
`preferably 1 to 10 (wt) %. The content of synthetic silicic acid with alkylsilylated
`silanol groups on the surface is an amount that can stabilize acephate, generally 1 to
`99 (wt) %.
`In addition to acephate and condensed sodium phosphate, a dry pesticide preparation
`using condensed sodium phosphate may further contain solid carriers for pesticide
`preparation in general. The solid carriers include, for example, mineral carriers such
`as kaolin, attapulgite, sericite, pyrophyllite, montmorillonite, zeolite, bentonite, acid
`clay, activated clay, serpentine, talc and diatomite, inorganic salts such as sulfate,
`nitrate, chloride and carbonate, inorganic carriers such as synthetic carriers (e.g.
`silica), or organic carriers such as sucrose, starch, dextrin, flour, soy flour, corn flour
`and wood flour.
`A dry pesticide preparation using synthetic silicic acid with alkylsilylated silanol
`groups on the surface in the present invention may comprise acephate and synthetic
`silicic acid with alkylsilylated silanol groups on the surface, but may further contain
`solid carriers for pesticide preparation. The solid carriers include the carriers
`mentioned above.
`The content of the solid carriers in the dry pesticide preparation can be generally 1 to
`90 (wt) %, preferably 20 to 70 (wt) %.
`A dry pesticide preparation in the present invention may contain adjuvants for
`pesticide preparation, for example at least one of surface active agents, coating agents,
`fragrance and known stabilizers, and their content is generally 0.1 to 35 (wt) %,
`preferably 2 to 10 (wt) %.
`Surface active agents that can be used in the present invention include for example
`anionic surface active agents, such as alkyl sulfates (e.g. sodium lauryl sulfate), alkyl
`arylsulfonate (e.g. sodium alkylnaphthalene sulfonate), lignin sulfonate (e.g. sodium
`lignosulfonate), succinate derivatives, polycarbonate, polyethylene glycol alkyl aryl
`ether sulfonate and aromatic sulfonate formaldehyde condensate, or nonionic surface
`active agents, such as polyoxyethylene alkyl ether, polyoxyethylene alkyl aryl ether
`and polyoxyethylene aryl aryl ether.
`A dry pesticide preparation in the present invention may further contain other
`insecticidal active ingredients, such as synthetic pyrethrin compounds, like
`Fenpropathrin, Fenvalerate and S-fenvalerate.
`A dry pesticide preparation in the present invention can be dustable powder, non-
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`floating dustable powder, wettable powder, water soluble powder, granule, water
`soluble granule, water dispersible granule, dry flowable, tablet or pill, and these dry
`pesticide preparations can be used by packaging them in packaging containers (e.g.
`water soluble packaging containers).
`A dry pesticide preparation in the present invention can be prepared by a conventional
`method, for example, mixing acephate and condensed sodium phosphate and/or
`synthetic silicic acid with alkylsilylated silanol groups on the surface in a mixer, if
`necessary additionally adding solid carriers and adjuvants (such as surface active
`agents), pulverizing the mixture by grinding mill, such as pneumatic grinding mill,
`hammer mill, jet mill and centrifugal mill, to an average particle size of 20 μm or less,
`thereby obtaining a powdery pesticide preparation as described in the present
`invention. In a further aspect, a compressive press such as roller compactor, extrusion
`granulator, plate granulator, fluidized bed granulator or roller pressing granulator, is
`used to mold the pulverized mixture, thereby obtaining a dry pesticide preparation as
`described in the present invention.
`Below the present invention will be described in detail with reference to the following
`preparation embodiments and test embodiments, but the present invention is not
`limited to these embodiments.
`
`Preparation embodiment 1
`Pulverize 25 parts by weight of acephate, 5 parts by weight of sodium
`tripolyphosphate, 4 parts by weight of sodium dodecylbenzene sulfonate, 2 parts by
`weight of aryl sulfonate sodium formaldehyde condensate, 20 parts by weight of
`Tokusil® GU-N (synthetic silicic acid produced by Tokuyama Soda) and 44 parts by
`weight of kaolin by jet mill, and mix the mixture in a mixer to obtain a dry pesticide
`preparation - wettable powder as described in the present invention.
`
`Preparation embodiment 2
`A dry pesticide preparation - wettable powder as described in the present invention is
`obtained according to preparation embodiment 1. Differently, 10 parts by weight of
`sodium tripolyphosphate is used to replace 5 parts by weight of sodium
`tripolyphosphate, and 39 parts by weight of kaolin is used to replace 44 parts by
`weight of kaolin.
`
`Preparation embodiment 3
`Pulverize 25 parts by weight of acephate, 20 parts by weight of Carplex® CS-701, 4
`parts by weight of sodium dodecylbenzene sulfonate, 2 parts by weight of aryl
`sulfonate sodium formaldehyde condensate and 49 parts by weight of kaolin by jet
`mill, and mix the mixture in a mixer to obtain a dry pesticide preparation - wettable
`powder as described in the present invention.
`
`Control preparation embodiment 1
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`Control preparation embodiment 1 proceeds according to preparation embodiment 1.
`Differently, 5 parts by weight of kaolin is used to replace 5 parts by weight of sodium
`tripolyphosphate.
`
`Control preparation embodiment 2
`Control preparation embodiment 2 proceeds according to preparation embodiment 3.
`Differently, 20 parts by weight of ToKusil® GU-N (synthetic silicic acid produced by
`ToKuyama Soda) is used to replace 20 parts by weight of Carplex® CS-701.
`
`Test embodiment
`The preparations obtained in the foregoing preparation embodiments and control
`preparation embodiments are sealed in aluminum laminated bags and stored in
`temperature controllable containers at specific temperature. The content of acephate is
`determined by gas chromatography before and after storage, and the decomposition
`rate is calculated according to the following formula:
`
`Decomposition rate (%) =100 – 100 ×
`
`Content of acephate after storage
`Content of acephate before storage
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`The results are shown in Table 2, Table 2 and Table 3.
`Table 1
`
`Tested preparation
`
`Decomposition rate (%)
`40 ℃
`
`Preparation embodiment 1
`Preparation embodiment 2
`Control preparation embodiment 1
`
`Tested preparation
`
`Preparation embodiment 1
`Preparation embodiment 2
`Control preparation embodiment 1
`
`After 1 month
`0
`1
`4
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`Table 2
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`After 3 months
`16
`13
`31
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`Decomposition rate (%)
`50 ℃
`
`After 2 weeks
`3
`2
`15
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`After 1 month
`26
`20
`44
`
`Table 3
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`Tested preparation
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`Preparation embodiment 3
`Control preparation embodiment 2
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`Decomposition rate (%)
`50 ℃
`
`After 2 weeks
`1
`6
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`After 1 month
`8
`33
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