CN117089022A - Preparation method of pyriproxyfen latex - Google Patents
Preparation method of pyriproxyfen latex Download PDFInfo
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- CN117089022A CN117089022A CN202311149292.0A CN202311149292A CN117089022A CN 117089022 A CN117089022 A CN 117089022A CN 202311149292 A CN202311149292 A CN 202311149292A CN 117089022 A CN117089022 A CN 117089022A
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- pyriproxyfen
- butadiene
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- 229920000126 latex Polymers 0.000 title claims abstract description 43
- 239000004816 latex Substances 0.000 title claims abstract description 42
- 239000005927 Pyriproxyfen Substances 0.000 title claims abstract description 19
- NHDHVHZZCFYRSB-UHFFFAOYSA-N pyriproxyfen Chemical compound C=1C=CC=NC=1OC(C)COC(C=C1)=CC=C1OC1=CC=CC=C1 NHDHVHZZCFYRSB-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title abstract description 13
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims abstract description 24
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000012071 phase Substances 0.000 claims abstract description 23
- 239000000839 emulsion Substances 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 21
- 239000008149 soap solution Substances 0.000 claims abstract description 20
- 239000003792 electrolyte Substances 0.000 claims abstract description 19
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims abstract description 18
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims abstract description 18
- 239000012874 anionic emulsifier Substances 0.000 claims abstract description 18
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 18
- 239000000194 fatty acid Substances 0.000 claims abstract description 18
- 229930195729 fatty acid Natural products 0.000 claims abstract description 18
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 18
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims abstract description 18
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008346 aqueous phase Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- KGIGUEBEKRSTEW-UHFFFAOYSA-N 2-vinylpyridine Chemical compound C=CC1=CC=CC=N1 KGIGUEBEKRSTEW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- -1 dicumyl hydroperoxide Chemical compound 0.000 claims abstract description 8
- 239000003999 initiator Substances 0.000 claims abstract description 8
- 239000000344 soap Substances 0.000 claims description 16
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 14
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 14
- 229910052700 potassium Inorganic materials 0.000 claims description 14
- 239000011591 potassium Substances 0.000 claims description 14
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 14
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- CFPHMAVQAJGVPV-UHFFFAOYSA-N 2-sulfanylbutanoic acid Chemical compound CCC(S)C(O)=O CFPHMAVQAJGVPV-UHFFFAOYSA-N 0.000 claims description 7
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 7
- 239000001103 potassium chloride Substances 0.000 claims description 7
- 235000011164 potassium chloride Nutrition 0.000 claims description 7
- 229910000160 potassium phosphate Inorganic materials 0.000 claims description 7
- 235000011009 potassium phosphates Nutrition 0.000 claims description 7
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 7
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 7
- 235000011151 potassium sulphates Nutrition 0.000 claims description 7
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 7
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 6
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 6
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 6
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 6
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 5
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 5
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 5
- FRQQKWGDKVGLFI-UHFFFAOYSA-N 2-methylundecane-2-thiol Chemical compound CCCCCCCCCC(C)(C)S FRQQKWGDKVGLFI-UHFFFAOYSA-N 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 8
- 238000003786 synthesis reaction Methods 0.000 abstract description 8
- 230000002159 abnormal effect Effects 0.000 abstract description 5
- 238000012797 qualification Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- YAJYJWXEWKRTPO-UHFFFAOYSA-N 2,3,3,4,4,5-hexamethylhexane-2-thiol Chemical compound CC(C)C(C)(C)C(C)(C)C(C)(C)S YAJYJWXEWKRTPO-UHFFFAOYSA-N 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- ADSOSINJPNKUJK-UHFFFAOYSA-N 2-butylpyridine Chemical compound CCCCC1=CC=CC=N1 ADSOSINJPNKUJK-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F236/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds
- C08F236/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds
- C08F236/04—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated
- C08F236/10—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated with vinyl-aromatic monomers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/28—Oxygen or compounds releasing free oxygen
- C08F4/32—Organic compounds
- C08F4/34—Per-compounds with one peroxy-radical
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention discloses a preparation method of pyriproxyfen latex. The preparation method of the butadiene-pyridine latex comprises the following steps: preparing a water phase pre-emulsion by a mixed system consisting of deionized water, rosin soap solution, fatty acid soap solution, an anionic emulsifier and electrolyte; mixing butadiene, styrene, 2-vinyl pyridine and a molecular weight regulator to prepare an oil phase solution; placing the aqueous phase pre-emulsion and the oil phase solution in a reaction container, dripping an initiator, and mixing and reacting at 20-30 ℃ to obtain the butadiene-pyridine latex; wherein the initiator is dicumyl hydroperoxide. The invention improves the current general formula of the pyriproxyfen latex, improves the original high-temperature synthesis at 50-60 ℃ to the low-temperature synthesis at 20-30 ℃ by forward progress of the propelling reaction, greatly improves the product qualification rate, effectively reduces the abnormal phenomenon in the production process, and further greatly improves the bonding capability of the finished latex.
Description
Technical Field
The invention belongs to the technical field of latex polymerization, and particularly relates to a preparation method of butadiene-pyridine latex.
Background
The butadiene-pyridine latex is widely used as a dipping adhesive for fiber cords, cord fabrics, ropes and the like which are framework materials of rubber products such as tires, rubber tubes, rubber tapes and the like in daily life, and the excellent adhesive property of the butadiene-pyridine latex is obviously superior to that of natural latex and other synthetic latex.
However, in the synthesis of the common butadiene-pyridine latex process, the self-organized glue connection is easy to occur due to the higher synthesis temperature, so that abnormal phenomena such as latex skinning and caking are easy to occur, the qualification rate of finished products in industrial production is lower, and further, the adhesive force is lower, the vulcanization is abnormal and the like.
Disclosure of Invention
The invention mainly aims to provide a preparation method of pyriproxyfen latex, which aims to overcome the defects in the prior art.
In order to achieve the above object, the technical solution adopted in the embodiment of the present invention includes:
the invention provides a preparation method of pyriproxyfen latex, which comprises the following steps:
preparing a water phase pre-emulsion by a mixed system consisting of deionized water, rosin soap solution, fatty acid soap solution, an anionic emulsifier and electrolyte;
mixing butadiene, styrene, 2-vinyl pyridine and a molecular weight regulator to prepare an oil phase solution;
placing the aqueous phase pre-emulsion and the oil phase solution in a reaction container, dripping an initiator, and mixing and reacting at 20-30 ℃ to obtain the butadiene-pyridine latex; wherein the initiator is dicumyl hydroperoxide.
Further, the aqueous phase pre-emulsion comprises 90% -95% of deionized water, 2% -3% of rosin soap solution, 2% -3% of fatty acid soap solution, 0.1% -1.5% of anionic emulsifier and 0.1% -1.5% of electrolyte.
Still further, the anionic emulsifier comprises any one or a combination of a plurality of rosin potassium soap, fatty acid potassium soap, sodium dodecyl benzene sulfonate or ammonium allyl polyoxyethylene ether sulfate.
Still further, the electrolyte comprises any one or a combination of potassium chloride, potassium sulfate, potassium phosphate, or sodium bicarbonate.
Further, the oil phase solution comprises 70-80% of butadiene, 10-20% of 2-vinyl pyridine, 0.5-1% of molecular weight regulator and 12-17% of styrene.
Still further, the molecular weight regulator comprises tertiary dodecyl mercaptan and/or mercaptobutyrate.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention improves the current general formula of the pyriproxyfen latex, improves the original high-temperature synthesis at 50-60 ℃ to the low-temperature synthesis at 20-30 ℃ by forward progress of the propelling reaction, greatly improves the product qualification rate, effectively reduces the abnormal phenomenon in the production process, and further greatly improves the bonding capability of the finished latex.
(2) The emulsion in the invention adopts a composite emulsifying system, promotes free radical polymerization under the initiation of dicumyl hydroperoxide, greatly excites a reactive system and ensures the normal reaction of the reaction at low temperature.
Detailed Description
In view of the defects in the prior art, the inventor provides a preparation method of the butadiene-pyridine latex through long-term research, and the method can greatly reduce the polymerization temperature of the butadiene-pyridine latex and reduce various anomalies caused by high temperature. The technical scheme, the implementation process, the principle and the like are further explained as follows.
One aspect of the embodiments of the present invention provides a method for preparing pyriproxyfen latex, comprising:
preparing a water phase pre-emulsion by a mixed system consisting of deionized water, rosin soap solution, fatty acid soap solution, an anionic emulsifier and electrolyte;
mixing butadiene, styrene, 2-vinyl pyridine and a molecular weight regulator to prepare an oil phase solution;
placing the aqueous phase pre-emulsion and the oil phase solution in a reaction container, dripping an initiator, and mixing and reacting at 20-30 ℃ to obtain the butadiene-pyridine latex; wherein the initiator is dicumyl hydroperoxide.
In some preferred embodiments, the aqueous pre-emulsion comprises 90% -95% deionized water, 2% -3% rosin soap, 2% -3% fatty acid soap, 0.1% -1.5% anionic emulsifier, and 0.1% -1.5% electrolyte.
In some more preferred embodiments, the anionic emulsifier may include any one or more combinations of rosin potassium soap, fatty acid potassium soap, sodium dodecylbenzene sulfonate, ammonium allylpolyoxyethylene ether sulfate, and the like, but is not limited thereto.
In some more preferred embodiments, the electrolyte may include any one or more combinations of potassium chloride, potassium sulfate, potassium phosphate, sodium bicarbonate, and the like, but is not limited thereto.
In some preferred embodiments, the oil phase solution comprises 70% -80% butadiene, 10% -20% 2-vinylpyridine, 0.5% -1% molecular weight regulator, and 12% -17% styrene.
In some more preferred embodiments, the molecular weight regulator may include, but is not limited to, t-dodecyl mercaptan and/or mercaptobutyrate.
According to the preparation method of the butyl pyridine latex, a novel initiating system is used in ternary polymerization emulsion formed by butadiene, styrene and 2-vinyl pyridine, and the forward progress of the reaction is further promoted by using additives such as an emulsifying agent, an electrolyte and the like, so that the butyl pyridine latex polymerization at a low temperature is completed.
The technical solution of the present invention will be described in further detail below with reference to a number of preferred embodiments, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. It should be noted that the examples described below are intended to facilitate the understanding of the present invention and are not intended to limit the present invention in any way. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The experimental methods, in which specific conditions are not noted in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer.
Example 1
The embodiment provides a preparation method of pyriproxyfen latex, which comprises the following steps:
(1) Preparing a mixed system consisting of 95 parts by weight of deionized water, 2.4 parts by weight of rosin soap solution, 2.4 parts by weight of fatty acid soap solution, 0.1 part by weight of anionic emulsifier and 0.1 part by weight of electrolyte into aqueous phase pre-emulsion; wherein the anionic emulsifier is any one or a combination of a plurality of rosin potassium soap, fatty acid potassium soap, sodium dodecyl benzene sulfonate, allyl polyoxyethylene ether ammonium sulfate and the like, and the electrolyte is any one or a combination of a plurality of potassium chloride, potassium sulfate, potassium phosphate, sodium bicarbonate and the like;
(2) Mixing 72 parts by weight of butadiene, 17 parts by weight of styrene, 10 parts by weight of 2-vinylpyridine and 1 part by weight of a molecular weight regulator to prepare an oil phase solution; wherein the molecular weight regulator is tert-dodecyl mercaptan and/or mercaptobutyrate;
(3) The aqueous phase pre-emulsion and the oil phase solution are placed in a reaction vessel, 0.2 weight part of dicumyl hydroperoxide is added dropwise, and the mixture is mixed and reacted under the condition of 20 to obtain the butadiene-pyridine latex.
Example 2
The embodiment provides a preparation method of pyriproxyfen latex, which comprises the following steps:
(1) Preparing a mixed system consisting of 91 parts by weight of deionized water, 3 parts by weight of rosin soap solution, 3 parts by weight of fatty acid soap solution, 1.5 parts by weight of anionic emulsifier and 1.5 parts by weight of electrolyte into aqueous phase pre-emulsion; wherein the anionic emulsifier is any one or a combination of a plurality of rosin potassium soap, fatty acid potassium soap, sodium dodecyl benzene sulfonate, allyl polyoxyethylene ether ammonium sulfate and the like, and the electrolyte is any one or a combination of a plurality of potassium chloride, potassium sulfate, potassium phosphate, sodium bicarbonate and the like;
(2) Mixing 74.5 parts by weight of butadiene, 15 parts by weight of styrene, 10 parts by weight of 2-vinylpyridine and 0.5 part by weight of a molecular weight regulator to prepare an oil phase solution; wherein the molecular weight regulator is tert-dodecyl mercaptan and/or mercaptobutyrate;
(3) The aqueous phase pre-emulsion and the oil phase solution are placed in a reaction vessel, 0.4 weight part of dicumyl hydroperoxide is added dropwise, and the mixture is mixed and reacted at the temperature of 25 ℃ to obtain the butadiene-pyridine latex.
Example 3
The embodiment provides a preparation method of pyriproxyfen latex, which comprises the following steps:
(1) Preparing a mixed system consisting of 94 parts by weight of deionized water, 2 parts by weight of rosin soap solution, 2 parts by weight of fatty acid soap solution, 1 part by weight of anionic emulsifier and 1 part by weight of electrolyte into aqueous phase pre-emulsion; wherein the anionic emulsifier is any one or a combination of a plurality of rosin potassium soap, fatty acid potassium soap, sodium dodecyl benzene sulfonate, allyl polyoxyethylene ether ammonium sulfate and the like, and the electrolyte is any one or a combination of a plurality of potassium chloride, potassium sulfate, potassium phosphate, sodium bicarbonate and the like;
(2) Mixing 72 parts by weight of butadiene, 12 parts by weight of styrene, 15 parts by weight of 2-vinylpyridine and 1 part by weight of a molecular weight regulator to prepare an oil phase solution; wherein the molecular weight regulator is tert-dodecyl mercaptan and/or mercaptobutyrate;
(3) The aqueous phase pre-emulsion and the oil phase solution are placed in a reaction vessel, 0.6 weight part of dicumyl hydroperoxide is added dropwise, and the mixture is mixed and reacted at the temperature of 30 ℃ to obtain the butadiene-pyridine latex.
Comparative example
The comparative example provides a preparation method of pyriproxyfen latex, which comprises the following steps:
(1) Preparing a mixed system consisting of 94 parts by weight of deionized water, 2 parts by weight of rosin soap solution, 2 parts by weight of fatty acid soap solution, 1 part by weight of anionic emulsifier and 1 part by weight of electrolyte into aqueous phase pre-emulsion; wherein the anionic emulsifier is any one or a combination of a plurality of rosin potassium soap, fatty acid potassium soap, sodium dodecyl benzene sulfonate, allyl polyoxyethylene ether ammonium sulfate and the like, and the electrolyte is any one or a combination of a plurality of potassium chloride, potassium sulfate, potassium phosphate, sodium bicarbonate and the like;
(2) Mixing 70 parts by weight of butadiene, 20 parts by weight of styrene, 9 parts by weight of 2-vinylpyridine and 1 part by weight of a molecular weight regulator to prepare an oil phase solution; wherein the molecular weight regulator is tert-dodecyl mercaptan and/or mercaptobutyrate;
(3) The aqueous phase pre-emulsion and the oil phase solution are placed in a reaction vessel, 0.8 weight part of potassium persulfate is added dropwise, and the mixture is mixed and reacted at the temperature of 60 ℃ to obtain the butadiene-pyridine latex.
The binding force of the butyl latices of examples 1-3 and comparative examples was tested according to GB/T9101-2002 test, comparing the following tables:
| adhesion test | Comparative example | Example 1 | Example 2 | Example 3 |
| Test 1 | 14.7 | 18.9 | 22.1 | 25.2 |
| Test 2 | 15.8 | 19.2 | 22.7 | 25.9 |
| Test 3 | 16.3 | 19.7 | 23.1 | 26.3 |
| Mean value of | 15.6 | 19.3 | 22.6 | 25.8 |
As can be seen from the table, the embodiment of the invention improves the current general formula of the pyriproxyfen latex, improves the original high-temperature synthesis at 50-60 ℃ to the low-temperature synthesis at 20-30 ℃ by forward progress of the propelling reaction, greatly improves the product qualification rate, effectively reduces the abnormal phenomenon in the production process, and further greatly improves the bonding capability of the finished latex.
In addition, the inventors have conducted experiments with other materials, process operations, and process conditions as described in this specification with reference to the foregoing examples, and have all obtained desirable results.
While the invention has been described with reference to an illustrative embodiment, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims. Moreover, unless specifically stated any use of the terms first, second, etc. do not denote any order or importance, but rather the terms first, second, etc. are used to distinguish one element from another.
Claims (6)
1. A method for preparing pyriproxyfen latex, comprising the steps of:
preparing a water phase pre-emulsion by a mixed system consisting of deionized water, rosin soap solution, fatty acid soap solution, an anionic emulsifier and electrolyte;
mixing butadiene, styrene, 2-vinyl pyridine and a molecular weight regulator to prepare an oil phase solution;
placing the aqueous phase pre-emulsion and the oil phase solution in a reaction container, dripping an initiator, and mixing and reacting at 20-30 ℃ to obtain the butadiene-pyridine latex; wherein the initiator is dicumyl hydroperoxide.
2. The method for preparing the pyriproxyfen latex according to claim 1, characterized in that: the aqueous phase pre-emulsion comprises 90-95% of deionized water, 2-3% of rosin soap solution, 2-3% of fatty acid soap solution, 0.1-1.5% of anionic emulsifier and 0.1-1.5% of electrolyte.
3. The method for preparing the pyriproxyfen latex according to claim 1 or 2, characterized in that: the anionic emulsifier comprises any one or a combination of a plurality of rosin potassium soap, fatty acid potassium soap, sodium dodecyl benzene sulfonate or allyl polyoxyethylene ether ammonium sulfate.
4. The method for preparing the pyriproxyfen latex according to claim 1 or 2, characterized in that: the electrolyte comprises any one or a combination of a plurality of potassium chloride, potassium sulfate, potassium phosphate or sodium bicarbonate.
5. The method for preparing the pyriproxyfen latex according to claim 1, characterized in that: the oil phase solution comprises 70-80% of butadiene, 10-20% of 2-vinyl pyridine, 0.5-1% of molecular weight regulator and 12-17% of styrene.
6. The method for preparing the pyriproxyfen latex according to claim 1 or 5, characterized in that: the molecular weight regulator comprises tertiary dodecyl mercaptan and/or mercaptobutyrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311149292.0A CN117089022A (en) | 2023-09-07 | 2023-09-07 | Preparation method of pyriproxyfen latex |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311149292.0A CN117089022A (en) | 2023-09-07 | 2023-09-07 | Preparation method of pyriproxyfen latex |
Publications (1)
| Publication Number | Publication Date |
|---|---|
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