CN115417893A - Production process of modified gamma-methacryloxypropyltrimethoxysilane - Google Patents
Production process of modified gamma-methacryloxypropyltrimethoxysilane Download PDFInfo
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- CN115417893A CN115417893A CN202211079540.4A CN202211079540A CN115417893A CN 115417893 A CN115417893 A CN 115417893A CN 202211079540 A CN202211079540 A CN 202211079540A CN 115417893 A CN115417893 A CN 115417893A
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- methacryloxypropyltrimethoxysilane
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- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical class CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000005086 pumping Methods 0.000 claims abstract description 27
- 159000000000 sodium salts Chemical class 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 22
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000012043 crude product Substances 0.000 claims abstract description 14
- SONHXMAHPHADTF-UHFFFAOYSA-M sodium;2-methylprop-2-enoate Chemical compound [Na+].CC(=C)C([O-])=O SONHXMAHPHADTF-UHFFFAOYSA-M 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 11
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- QLCFPDLVOCOPON-UHFFFAOYSA-N CCC(CO)(CO)CO.CC(O)COC(C)COC(C)CO Chemical compound CCC(CO)(CO)CO.CC(O)COC(C)COC(C)CO QLCFPDLVOCOPON-UHFFFAOYSA-N 0.000 claims abstract description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000007921 spray Substances 0.000 claims description 31
- 239000000463 material Substances 0.000 claims description 26
- 238000005192 partition Methods 0.000 claims description 19
- 239000002904 solvent Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000000428 dust Substances 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 9
- 239000007822 coupling agent Substances 0.000 claims description 7
- 239000003112 inhibitor Substances 0.000 claims description 7
- 238000006116 polymerization reaction Methods 0.000 claims description 7
- 238000001694 spray drying Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- OXYZDRAJMHGSMW-UHFFFAOYSA-N 3-chloropropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCl OXYZDRAJMHGSMW-UHFFFAOYSA-N 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 5
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 230000000149 penetrating effect Effects 0.000 claims description 5
- 238000006011 modification reaction Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical group CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 2
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 2
- RKHXQBLJXBGEKF-UHFFFAOYSA-M tetrabutylphosphanium;bromide Chemical group [Br-].CCCC[P+](CCCC)(CCCC)CCCC RKHXQBLJXBGEKF-UHFFFAOYSA-M 0.000 claims description 2
- 125000004122 cyclic group Chemical group 0.000 claims 2
- 230000004888 barrier function Effects 0.000 claims 1
- 239000012948 isocyanate Substances 0.000 abstract description 6
- 150000002513 isocyanates Chemical class 0.000 abstract description 6
- 238000004383 yellowing Methods 0.000 abstract description 4
- 229920002635 polyurethane Polymers 0.000 abstract description 3
- 239000004814 polyurethane Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000004821 distillation Methods 0.000 description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 239000006087 Silane Coupling Agent Substances 0.000 description 4
- 238000007790 scraping Methods 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 229920001730 Moisture cure polyurethane Polymers 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000002912 waste gas Substances 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241000122235 Junco hyemalis Species 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000002318 adhesion promoter Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 239000002981 blocking agent Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- -1 glycol ether modified gamma-methacryloxypropyltrimethoxysilane Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910003471 inorganic composite material Inorganic materials 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000007348 radical reaction Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/16—Evaporating by spraying
- B01D1/18—Evaporating by spraying to obtain dry solids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/1892—Preparation; Treatments not provided for in C07F7/20 by reactions not provided for in C07F7/1876 - C07F7/1888
Abstract
The invention belongs to the field of organic synthesis, and particularly relates to a production process of modified gamma-methacryloxypropyltrimethoxysilane, which comprises the following steps: s1, sodium salt synthesis procedure: pumping methacrylic acid and water into a sodium salt synthesis kettle, starting stirring, dropwise adding a sodium hydroxide solution with the mass fraction of 30-40%, controlling the temperature of the kettle to be not more than 60 ℃, continuously stirring for 2-4h, and pumping a sodium methacrylate crude product into a sodium salt crude product tank when the pH of the solution in the kettle is = 7-9; s2, drying of sodium salt: s3, a synthesis process: and (4) modifying gamma-methacryloxypropyltrimethoxysilane. The beneficial effects are that: the preparation method of the modified gamma-methacryloxypropyl trimethoxy silane prepared by the invention is simple and easy to implement, the raw materials are easy to obtain, and the reaction process of the amino-terminated trimethylolpropane tripropylene glycol ether modified gamma-methacryloxypropyl trimethoxy silane with polyurethane isocyanate prepolymer is easy to control, gel phenomenon can not be generated, and yellowing can not occur.
Description
Technical Field
The invention belongs to the field of organic synthesis, and particularly relates to a production process of modified gamma-methacryloxypropyltrimethoxysilane.
Background
Silane coupling agents are a class of organosilicon compounds that contain two different chemical groups in the molecule. The silane coupling agent generally has a molecular formula of Y-R-Si (OR) 3 (wherein Y-organic functional group, siOR-siloxy). The siloxy group is reactive with inorganic species and the organofunctional group is reactive or compatible with organic species. Thus, when a silane coupling agent is interposed between the inorganic and organic interfaces, a bonding layer of organic matrix-silane coupling agent-inorganic matrix may be formed. Due to the special structure, the organic silicon/inorganic composite material has a reaction group capable of being chemically combined with inorganic materials (such as glass, silica sand, metal and the like) and a reaction group capable of being chemically combined with organic materials (such as synthetic resin and the like) in a molecule, can be used for surface treatment, and can also be used as an adhesion promoter of a sealant and an adhesive.
Gamma-methacryloxypropyltrimethoxysilane is an organofunctional silane coupling agent and can improve the mechanical and electrical properties of thermosetting resins containing inorganic fillers, particularly thermoplastic resins cured by reactive free radical reaction (such as unsaturated polyesters, polyurethanes and acrylates). However, when the gamma-methacryloxypropyltrimethoxysilane is used as a blocking agent to carry out blocking modification on the isocyanate polyurethane prepolymer, the phenomena of gelation and yellowing are easy to occur, and the whole reaction process is not easy to control.
Therefore, the invention improves the defects by modifying gamma-methacryloxypropyltrimethoxysilane by using the amino-terminated trimethylolpropane tripropylene glycol ether.
The invention also provides a modified gamma-methacryloxypropyl trimethoxy silane process route, the inventor improves the spray dryer, the Chinese utility model patent with the publication number of CN203598504U discloses 'a spray dryer', the dryer comprises a spray head, a suction roller, a body, a scraping partition plate, a hot air inlet, a dust cover and a waste gas outlet, the body is a sealed cavity which is vertically placed in a cylindrical structure, the center of the surface of the top of the body is provided with the spray head, the hot inlet is arranged on the side wall of the body and slightly lower than the spray head, the lower end of the hot air inlet is provided with the scraping partition plate which is horizontally fixed, the scraping partition plate covers the side wall of the body at the symmetrical position of the hot air inlet, the symmetrical position is provided with a long opening, the suction roller is horizontally arranged at the opening, one side of the suction roller is attached to the edge of the scraping partition plate, the other side of the suction roller is close to the side wall of the body, the waste gas outlet is arranged on the top of the side wall of the top of the body at the right upper end of the hot air inlet, and the periphery of the waste gas outlet is coated with the dust cover; the hot air of the dryer enters the cavity through the single hot air inlet, and uniform drying is not facilitated.
Therefore, the inventor provides a production process of modified gamma-methacryloxypropyl trimethoxysilane by taking the experience of abundant design development and actual manufacturing of related industries for years as a basis and researching and improving the existing structure and deficiency, so as to achieve the purpose of higher practical value.
Disclosure of Invention
In order to solve the problems, the invention provides a production process of modified gamma-methacryloxypropyltrimethoxysilane.
The invention provides the following technical scheme:
a production process of modified gamma-methacryloxypropyl trimethoxy silane comprises the following steps:
s1, sodium salt synthesis procedure:
pumping methacrylic acid and water into a sodium salt synthesis kettle, starting stirring, dropwise adding a sodium hydroxide solution with the mass fraction of 30-40%, controlling the temperature of the kettle to be not more than 60 ℃, continuously stirring for 2-4h, and pumping a sodium methacrylate crude product into a sodium salt crude product tank when the pH of the solution in the kettle is = 7-9;
s2, drying of sodium salt:
stirring the materials in the sodium salt crude product tank, putting the materials into a sodium salt cooling kettle, pumping the materials into a spray drying system for drying, keeping the air inlet temperature between 180 and 230 ℃ and the air outlet temperature between 80 and 120 ℃, and drying to obtain a finished product of sodium methacrylate;
s3, a synthesis process:
pumping chloropropyl trimethoxyl silane into a coupling agent synthesis kettle, heating to 60-70 ℃, pumping a solvent, and heating to 90-100 ℃; pumping sodium methacrylate and a polymerization inhibitor into a sodium salt feeding tank, then pushing the sodium methacrylate and the polymerization inhibitor into a coupling agent synthesis kettle through a screw, simultaneously adding a metered catalyst, heating to about 110-120 ℃, reacting for 3-4h, and after the reaction is finished, centrifuging and distilling to obtain a finished product of gamma-methacryloxypropyltrimethoxysilane;
s4, modification of gamma-methacryloxypropyltrimethoxysilane:
pumping the finished product of the gamma-methacryloxypropyltrimethoxysilane and DMF into a modification reaction kettle, introducing nitrogen for stirring, dripping amino-terminated trimethylolpropane tripolypropylene glycol ether at the temperature of 40-50 ℃, heating to 60-70 ℃, preserving the temperature for reaction for 6-8h, and performing post-treatment after the reaction is finished to obtain the modified gamma-methacryloxypropyltrimethoxysilane.
Preferably, the polymerization inhibitor is 2, 6-di-tert-butyl-4-methylphenol; the catalyst is tetrabutyl phosphonium bromide.
Preferably, the feeding molar ratio of the gamma-methacryloxypropyltrimethoxysilane to the amino-terminated trimethylolpropane tripolypropylene glycol ether is 1:1.
Spray drying system includes spray dryer, high-speed centrifugal atomizer, cyclone, sack cleaner and draught fan, high-speed centrifugal atomizer sets up in spray dryer's top, and high-speed centrifugal atomizer's one end and inlet pipe intercommunication connect gradually through the pipeline between spray dryer, cyclone, sack cleaner and the draught fan, spray dryer's interior roof is provided with annular air partition plate, and annular air partition plate divide into interior cavity and outer cavity with spray dryer's inside, and the upper end wall of outer cavity evenly encircles and has seted up a plurality of groups of branch pipes, and the one end intercommunication of branch pipe has annular distributor, and annular distributor's lateral wall is connected with the air-supply line, the air-supply line has set gradually air cleaner, air-blower and heater along the air inlet direction from the air inlet end.
Preferably, the roof of interior chamber is equipped with annular turning block, and annular turning block joint is in the roof annular groove of interior chamber, the bottom of annular turning block is provided with a connecting rod of a plurality of groups along edge ring, and the bottom slope of a connecting rod is provided with the connecting rod No. two, and the one end that a connecting rod was kept away from to the connecting rod No. two is connected with the main shaft perpendicularly, and the outer wall of main shaft is provided with the stirring wheel.
Preferably, the outer wall of the first connecting rod is provided with a circle of annular limiting slide block, and the annular limiting slide block extends towards the side wall of the annular air partition plate; the side wall of the annular air partition plate is provided with an annular limiting sliding groove corresponding to the annular limiting sliding block.
Preferably, the outer wall of the annular rotating block is uniformly provided with a plurality of groups of teeth in a surrounding manner, the teeth are meshed with a main gear, the inner wall of the main gear is connected with a motor through a rotating shaft, and the motor is arranged on one side of the top of the spray dryer.
Preferably, the bottom of the spray dryer is communicated with a hopper, a blanking valve is arranged at the bottom of the hopper, a first air-lock valve is arranged at the bottom of the cyclone separator, and a second air-lock valve is arranged at the bottom of the bag-type dust collector.
Preferably, the annular air partition plate is divided into an upper end part and a lower end part, the lower end part is open, the cross section area of the lower end part is smaller than that of the upper end part, and the stirring wheels are distributed on two side walls of the main shaft at equal intervals.
Preferably, the bottom of the main shaft is fixedly connected with a rotating shaft through a connecting shaft, the rotating shaft extends towards a fixed rod on the inner wall of the hopper, and a stop block is arranged at the end, penetrating through the fixed rod, of the rotating shaft, extending downwards;
the outer wall of axis of rotation is provided with helical blade, the inner wall of axis of rotation is equipped with the air inlet cavity, and the both sides wall intercommunication of air inlet cavity has the multiunit intercommunication pipeline, and the intercommunication pipeline extends to helical blade's last wall and link up, and link up the department and be provided with the filter screen.
Preferably, the lower end opening of the air inlet cavity is inserted with an air inlet pipe, the air inlet pipe penetrates through the stop block and extends outwards, and the end is connected with an air heater
The beneficial effects of the invention are:
1. compared with the prior art, the modified gamma-methacryloxypropyltrimethoxysilane prepared by the invention has the advantages of simple and easy preparation method, easily obtained raw materials and low price, and the reaction process of the amino-terminated trimethylolpropane tripolypropylene glycol ether modified gamma-methacryloxypropyltrimethoxysilane and the isocyanate polyurethane prepolymer is easy to control, gel phenomenon can not be generated, and yellowing can not occur.
2. According to the invention, the annular air partition plate is arranged, the interior of the spray dryer is divided into the inner chamber and the outer chamber, and the main shaft and the stirring wheel are arranged at the same time, so that a certain negative pressure is formed when the stirring wheel rotates rapidly, and therefore, the hot air can be guided and adsorbed, the hot air can continuously move upwards and fully contact with the materials, and the drying effect is improved.
In conclusion, the invention overcomes the defects of the prior art, has reasonable design and compact structure, and has higher social use value and application prospect.
Drawings
FIG. 1 is a schematic diagram of the spray drying system of the present invention;
FIG. 2 is a schematic view of the spray dryer of the present invention;
FIG. 3 is a schematic view of the installation structure of the annular rotating block of the present invention;
FIG. 4 is a schematic diagram of the structure of the ring distributor of the present invention;
FIG. 5 is an enlarged view of the structure A of the present invention;
FIG. 6 is an enlarged view of the structure B of the present invention.
In the figure: a spray dryer 1, an air filter 101, a blower 102, an air inlet pipe 103, a heater 104, an annular distributor 105, and a branch pipe 106;
the device comprises an annular air partition plate 11, a first connecting rod 12, a second connecting rod 13, a main shaft 14, a stirring wheel 15, an annular rotating block 16, an annular limiting sliding block 17, a main gear 18, a motor 19, a connecting shaft 20, a rotating shaft 21, a fixing rod 22, a stop block 23, an air inlet cavity 24, a communicating pipeline 25, a filter screen 26, an air inlet pipe 27, a hot air blower 28, a spiral blade 29 and a hopper 30;
the device comprises a high-speed centrifugal atomizer 2, a cyclone separator 3, a bag-type dust collector 4, an induced draft fan 5, a blanking valve 6, a first air-lock valve 7 and a second air-lock valve 8.
Detailed Description
The present invention will be specifically described below with reference to specific examples.
Example 1
A production process of modified gamma-methacryloxypropyltrimethoxysilane comprises the following steps:
s1, sodium salt synthesis procedure:
pumping methacrylic acid and water into a sodium salt synthesis kettle, starting stirring, dropwise adding a sodium hydroxide solution with the mass fraction of 30-40%, controlling the temperature of the kettle to be not more than 60 ℃, continuously stirring for 3h, and pumping a sodium methacrylate crude product into a sodium salt crude product tank when the pH of the solution in the kettle is = 7-9;
the molar ratio of methacrylic acid to sodium hydroxide was 1:1.
S2, drying of sodium salt:
and (3) stirring the materials in the sodium salt crude product tank, putting the materials into a sodium salt cooling kettle, pumping the materials into a spray drying system through a Mono pump for drying, keeping the air inlet temperature at about 190 ℃ and the air outlet temperature at about 90 ℃, and drying to obtain a finished product of sodium methacrylate for the next procedure.
S3, a synthesis process:
pumping chloropropyltrimethoxysilane into a workshop metering tank from a tank storage tank, adding the chloropropyltrimethoxysilane into a coupling agent synthesis kettle through a metering pump, and heating to about 70 ℃; pumping the solvent into a feeding tank from a centralized feeding area, then pumping the solvent into a synthesis kettle, and heating to about 90 ℃; conveying the sodium methacrylate from the sodium salt temporary storage tank to a sodium salt feeding tank in vacuum, pumping a polymerization inhibitor into the sodium salt feeding tank, pushing the sodium methacrylate into a coupling agent synthesis kettle through a screw, adding a metered catalyst, heating to about 120 ℃, keeping the temperature and reacting for 3 hours, and finishing the reaction;
the mol ratio of the sodium methacrylate to the chloropropyltrimethoxysilane is 1.
S4, a centrifugation process:
after the reaction is finished, pumping the materials in the coupling agent synthesis kettle into a cooling kettle, cooling to about 60 ℃, dropping the materials into a centrifuge through a closed pipeline by utilizing self weight, separating a gamma-methacryloxypropyl trimethoxy silane crude product and sodium chloride through the centrifuge, feeding the gamma-methacryloxypropyl trimethoxy silane crude product into a distillation section, leaching the sodium chloride in the centrifuge by adopting a solvent, feeding the washed and centrifuged sodium chloride into a wet salt drying section, collecting the solvent, feeding the solvent into a washing receiving tank, and pumping the solvent into a purification distillation kettle of an auxiliary workshop for normal pressure distillation;
s5, a distillation process:
transferring the crude product of gamma-methacryloxypropyltrimethoxysilane to a distillation kettle through a tundish, controlling the vacuum in the kettle to be-0.095 MPa at the initial stage, heating the distillation kettle, collecting materials with the kettle temperature of about 100 ℃ as a solvent, and recycling the materials; after the solvent is distilled, controlling the vacuum in the distillation kettle to be-0.098 MPa, gradually heating the distillation kettle to 130 ℃, and cooling circulating water to obtain a finished product of the gamma-methacryloxypropyltrimethoxysilane. Then pumping into a rectifying still for refining;
s6, drying wet salt:
the sodium chloride after washing and centrifugation is automatically scraped off by a centrifuge, and is pumped into a vacuum rake dryer through a solid feeding machine, the vacuum of the rake dryer is controlled to be-0.098 MPa, the temperature is gradually increased, the pressure is reduced and the drying is carried out for 3h when the temperature of the kettle is 120 ℃, the solvent is condensed and recovered, the solvent is collected and enters a solvent receiving tank, and the solvent is pumped into an auxiliary workshop purification distillation kettle.
S7, modification of gamma-methacryloxypropyltrimethoxysilane:
pumping the finished product of the gamma-methacryloxypropyl trimethoxysilane into a modification reaction kettle by using a solvent, introducing nitrogen for stirring, dropwise adding amino-terminated trimethylolpropane tripolypropylene glycol ether at 50 ℃, heating to 65 ℃, preserving the temperature for reaction for 7 hours, and distilling and refining after the reaction is finished to obtain the modified gamma-methacryloxypropyl trimethoxysilane.
The feeding molar ratio of the gamma-methacryloxypropyltrimethoxysilane to the amino-terminated trimethylolpropane tripolypropylene glycol ether is 1:1.
The solvent used in the present invention is not particularly limited, and DMF is used.
Performance detection
Modified gamma-methacryloxypropyltrimethoxysilane obtained in example 1 was reacted with a polyurethane isocyanate prepolymer (Trixene SC7702 shanghai junko materials science and technology ltd) in a silane to isocyanate molar ratio of 1:1, reacting for 5 hours at 60 ℃ in a nitrogen atmosphere; the reaction is finished when no isocyanate exists, so that the modified gamma-methacryloxypropyltrimethoxysilane polyurethane prepolymer is obtained, and no gel or yellowing phenomenon is generated in the whole detection process.
Example 2
Referring to fig. 1-4, the spray drying system comprises a spray dryer 1, a high-speed centrifugal atomizer 2, a cyclone separator 3, a bag-type dust collector 4 and an induced draft fan 5, wherein the high-speed centrifugal atomizer 2 is arranged at the top of the spray dryer 1, one end of the high-speed centrifugal atomizer 2 is communicated with a feeding pipe, the spray dryer 1, the cyclone separator 3, the bag-type dust collector 4 and the induced draft fan 5 are sequentially connected through a pipeline, an annular air partition plate 11 is arranged on the inner top wall of the spray dryer 1, the annular air partition plate 11 is divided into an upper end part and a lower end part, the lower end part is open, the cross sectional area of the lower end part is smaller than that of the upper end part, the retention time of atomized materials in an inner cavity is prolonged, and further drying is facilitated;
the material to be dried enters the high-speed centrifugal atomizer 2 through a pipeline for atomization, the air blower 102 is started at the same time, the outside air is firstly filtered by the air filter 101, then is heated by the heater 104, enters the annular distributor 105 for distribution, enters the branch pipe 106, and then enters the spray dryer 1 for drying the atomized material;
the inside of the spray dryer 1 is divided into an inner chamber and an outer chamber by the annular air partition plate 11, a plurality of groups of branch pipes 106 are uniformly arranged on the upper end wall of the outer chamber in a surrounding manner, one end of each branch pipe 106 is communicated with an annular distributor 105, the side wall of each annular distributor 105 is connected with an air inlet pipe 103, and the air inlet pipe 103 is sequentially provided with an air filter 101, an air blower 102 and a heater 104 from an air inlet end along an air inlet direction.
The top wall of the inner chamber is provided with an annular rotating block 16, the annular rotating block 16 is clamped in an annular groove of the top wall of the inner chamber, the bottom of the annular rotating block 16 is provided with a plurality of groups of first connecting rods 12 in a surrounding manner along the edge, the bottom of each first connecting rod 12 is obliquely provided with a second connecting rod 13, one end, far away from the first connecting rod 12, of the second connecting rod 13 is vertically connected with a main shaft 14, the outer wall of the main shaft 14 is provided with a stirring wheel 15, the stirring wheel 15 is equidistantly distributed on two side walls of the main shaft 14, the outer wall of the annular rotating block 16 is uniformly provided with a plurality of groups of teeth in a surrounding manner and is connected with a main gear 18 through meshing of the teeth, the inner wall of the main gear 18 is connected with a motor 19 through a rotating shaft, and the motor 19 is installed on one side of the top of the spray dryer 1;
the bottom of the main shaft 14 is fixedly connected with a rotating shaft 21 through a connecting shaft 20, the rotating shaft 21 extends towards a fixed rod 22 on the inner wall of a hopper 30, a stop block 23 is arranged at the end, extending downwards, of the rotating shaft 21, penetrating through the fixed rod 22, the stop block 23 supports and limits the rotating shaft 21 to a certain extent, a spiral blade 29 is arranged on the outer wall of the rotating shaft 21, an air inlet cavity 24 is arranged on the inner wall of the rotating shaft 21, two side walls of the air inlet cavity 24 are communicated with a plurality of groups of communicating pipelines 25, the communicating pipelines 25 extend and penetrate towards the upper wall of the spiral blade 29, a filter screen 26 is arranged at the penetrating position to prevent materials from entering the air inlet cavity 24, an air inlet pipe 27 is inserted into an opening at the lower end of the air inlet cavity 24, and the end, extending outwards, penetrating through the stop block 23, of the air inlet pipe 27 is connected with an air heater 28;
the motor 19 drives the rotating shaft 21 to rotate and drives the materials to continuously push upwards through the helical blades 29, so that the materials can be turned to the maximum extent, the contact area of the materials and hot air is increased, and the drying effect is improved; meanwhile, the hot air blower 28 is started, hot air enters the communicating pipeline 25 through the air inlet pipe 27 and is discharged upwards through the filter screen 26 on the upper surface wall of the helical blade 29, and therefore the atomized materials are further dried;
the motor 19 drives the main gear 18 to rotate through a rotating shaft, the main gear 18 drives the annular rotating block 16 to rotate, and drives the stirring wheel 15 to rotate through the first connecting rod 12, the second connecting rod 13 and the main shaft 14, and the rotation is carried out in the inner chamber of the spray dryer 1, so that a certain negative pressure can be formed when the stirring wheel 15 rotates, and hot air in the outer chamber can enter the inner chamber along the annular air partition plate 11, so that the hot air can be fully contacted with atomized materials, and the drying treatment can be carried out to a greater extent;
the outer wall of the first connecting rod 12 is provided with a circle of annular limiting sliding blocks 17, and the annular limiting sliding blocks 17 extend towards the side wall of the annular air partition plate 11; the side wall of the annular air partition plate 11 is provided with an annular limiting sliding groove corresponding to the annular limiting sliding block 17, and the annular limiting sliding groove limits the annular limiting sliding block 17, so that the stable rotation of the annular limiting sliding block 17 is ensured;
the bottom of the spray dryer 1 is provided with a blanking valve 6, the bottom of the cyclone separator 3 is provided with a first air-lock valve 7, the bottom of the bag-type dust remover 4 is provided with a second air-lock valve 8, most of materials after drying treatment are discharged outwards through the blanking valve 6, and other materials are subjected to dust removal and adsorption through the cyclone separator 3 and the bag-type dust remover 4 in sequence under the action of the induced draft fan 5 and finally discharged outwards through the first air-lock valve 7 and the second air-lock valve 8.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (11)
1. A production process of modified gamma-methacryloxypropyltrimethoxysilane is characterized by comprising the following steps:
s1, sodium salt synthesis procedure:
pumping methacrylic acid and water into a sodium salt synthesis kettle, starting stirring, dropwise adding a sodium hydroxide solution with the mass fraction of 30-40%, controlling the temperature of the kettle to be not more than 60 ℃, continuously stirring for 2-4h, and pumping a sodium methacrylate crude product into a sodium salt crude product tank when the pH of the solution in the kettle is = 7-9;
s2, drying of sodium salt:
stirring the materials in the sodium salt crude product tank, putting the materials into a sodium salt cooling kettle, pumping the materials into a spray drying system for drying, keeping the air inlet temperature between 180 and 230 ℃ and the air outlet temperature between 80 and 120 ℃, and drying to obtain a finished product of sodium methacrylate;
s3, a synthesis process:
pumping chloropropyl trimethoxyl silane into a coupling agent synthesis kettle, heating to 60-70 ℃, pumping a solvent, and heating to 90-100 ℃; pumping sodium methacrylate and a polymerization inhibitor into a sodium salt feeding tank, then pushing the sodium methacrylate and the polymerization inhibitor into a coupling agent synthesis kettle through a screw, simultaneously adding a metered catalyst, heating to about 110-120 ℃, reacting for 3-4h, and after the reaction is finished, centrifuging and distilling to obtain a finished product of gamma-methacryloxypropyl trimethoxy silane;
s4, modification of gamma-methacryloxypropyltrimethoxysilane:
pumping the finished product of the gamma-methacryloxypropyltrimethoxysilane and DMF into a modification reaction kettle, introducing nitrogen for stirring, dripping amino-terminated trimethylolpropane tripolypropylene glycol ether at the temperature of 40-50 ℃, heating to 60-70 ℃, preserving the temperature for reaction for 6-8h, and performing post-treatment after the reaction is finished to obtain the modified gamma-methacryloxypropyltrimethoxysilane.
2. The process for producing modified gamma-methacryloxypropyltrimethoxysilane according to claim 1, wherein the polymerization inhibitor is 2, 6-di-tert-butyl-4-methylphenol; the catalyst is tetrabutyl phosphonium bromide.
3. The process for producing modified gamma-methacryloxypropyltrimethoxysilane according to claim 1, wherein the molar ratio of the gamma-methacryloxypropyltrimethoxysilane to the amino-terminated trimethylolpropane tripropylene glycol ether is 1:1.
4. The production process of the modified gamma-methacryloxypropyltrimethoxysilane according to claim 1, wherein the spray drying system comprises a spray dryer (1), a high-speed centrifugal atomizer (2), a cyclone separator (3), a bag-type dust collector (4) and an induced draft fan (5), the high-speed centrifugal atomizer (2) is arranged at the top of the spray dryer (1), one end of the high-speed centrifugal atomizer (2) is communicated with the feeding pipe, and the spray dryer (1), the cyclone separator (3), the bag-type dust collector (4) and the induced draft fan (5) are sequentially connected through a pipeline, and the production process is characterized in that:
the interior roof of spray dryer (1) is provided with cyclic annular air baffle (11), and cyclic annular air baffle (11) divide into the inside of spray dryer (1) inner chamber and outer cavity, and a plurality of groups branch pipe (106) have evenly been encircleed to the upper end wall of outer cavity, and the one end intercommunication of branch pipe (106) has annular distributor (105), and the lateral wall of annular distributor (105) is connected with air-supply line (103), air-supply line (103) have set gradually air cleaner (101), air-blower (102) and heater (104) along the air inlet direction from the air inlet end.
5. The production process of modified gamma-methacryloxypropyltrimethoxysilane according to claim 4, wherein an annular rotating block (16) is arranged on the top wall of the inner chamber, the annular rotating block (16) is clamped in an annular groove on the top wall of the inner chamber, a plurality of groups of first connecting rods (12) are arranged at the bottom of the annular rotating block (16) along the edge in a surrounding manner, a second connecting rod (13) is obliquely arranged at the bottom of the first connecting rod (12), a main shaft (14) is vertically connected to one end, away from the first connecting rod (12), of the second connecting rod (13), and a stirring wheel (15) is arranged on the outer wall of the main shaft (14).
6. The production process of modified gamma-methacryloxypropyltrimethoxysilane according to claim 4, wherein the outer wall of the first connecting rod (12) is provided with a ring of annular limiting slide blocks (17), and the annular limiting slide blocks (17) extend towards the side wall of the annular air partition plate (11); the side wall of the annular air partition plate (11) is provided with an annular limiting sliding groove corresponding to the annular limiting sliding block (17).
7. The process for producing modified gamma-methacryloxypropyltrimethoxysilane according to claim 5, wherein the outer wall of the annular rotating block (16) is uniformly provided with a plurality of sets of teeth in a surrounding manner, a main gear (18) is connected to the outer wall of the annular rotating block through the engagement of the teeth, the inner wall of the main gear (18) is connected with a motor (19) through a rotating shaft, and the motor (19) is installed on one side of the top of the spray dryer (1).
8. The production process of modified gamma-methacryloxypropyltrimethoxysilane according to claim 4, wherein the bottom of the spray dryer (1) is communicated with a hopper (30), the bottom of the hopper (30) is provided with a blanking valve (6), the bottom of the cyclone separator (3) is provided with a first air shutter (7), and the bottom of the bag-type dust collector (4) is provided with a second air shutter (8).
9. The process for producing modified gamma-methacryloxypropyltrimethoxysilane according to claim 6, wherein the annular air barrier (11) is divided into an upper end and a lower end, the lower end is open, and the cross-sectional area of the lower end is smaller than that of the upper end.
10. The process for producing modified gamma-methacryloxypropyltrimethoxysilane according to claim 5, wherein a rotating shaft (21) is fixedly connected to the bottom of the main shaft (14) through a connecting shaft (20), the rotating shaft (21) extends towards a fixing rod (22) on the inner wall of the hopper (30), and a stop block (23) is arranged at the end of the rotating shaft (21) penetrating through the fixing rod (22) and extending downwards;
the outer wall of axis of rotation (21) is provided with helical blade (29), the inner wall of axis of rotation (21) is equipped with air inlet cavity (24), and the both sides wall intercommunication of air inlet cavity (24) has multiunit communicating pipe (25), and communicating pipe (25) extend to the last wall of helical blade (29) and link up, and link up the department and be provided with filter screen (26).
11. The production process of modified gamma-methacryloxypropyltrimethoxysilane according to claim 10, wherein an air inlet pipe (27) is inserted into the opening at the lower end of the air inlet cavity (24), and the end of the air inlet pipe (27) extending outwards through the stop block (23) is connected with an air heater (28).
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| JP2004339170A (en) * | 2003-05-16 | 2004-12-02 | Nippon Shokubai Co Ltd | (meth)acrylic acid alkali metal salt and method for producing the same |
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| JP2004339170A (en) * | 2003-05-16 | 2004-12-02 | Nippon Shokubai Co Ltd | (meth)acrylic acid alkali metal salt and method for producing the same |
| CN105061487A (en) * | 2015-08-07 | 2015-11-18 | 荆州市江汉精细化工有限公司 | Method for producing methacryloxypropyltrimethoxysilane |
| CN105273371A (en) * | 2015-11-05 | 2016-01-27 | 东华大学 | Thermoplastic polyester composition and preparation method thereof |
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Denomination of invention: A modified g- Production process of methacryloxypropyltrimethoxysilane Granted publication date: 20230530 Pledgee: Agricultural Bank of China Limited Hexian Branch Pledgor: ANHUI GB SILICONES NEW MATERIAL CO.,LTD. Registration number: Y2024980011591 |