CN117887414A - Organic silica gel adhesive - Google Patents
Organic silica gel adhesive Download PDFInfo
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- CN117887414A CN117887414A CN202410185134.9A CN202410185134A CN117887414A CN 117887414 A CN117887414 A CN 117887414A CN 202410185134 A CN202410185134 A CN 202410185134A CN 117887414 A CN117887414 A CN 117887414A
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- Prior art keywords
- carbon black
- white carbon
- calcium carbonate
- stirring
- modified
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 180
- 239000000853 adhesive Substances 0.000 title claims abstract description 50
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 50
- 239000000741 silica gel Substances 0.000 title claims abstract description 44
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 44
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 140
- 239000006229 carbon black Substances 0.000 claims abstract description 94
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 70
- 238000002360 preparation method Methods 0.000 claims abstract description 55
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 7
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims abstract description 6
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims abstract description 6
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims abstract description 6
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims description 42
- 229960001545 hydrotalcite Drugs 0.000 claims description 42
- 229910001701 hydrotalcite Inorganic materials 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 35
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 30
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 30
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 30
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims description 27
- AXTPGQHJFRSSQJ-UHFFFAOYSA-N dichloro-ethoxy-methylsilane Chemical compound CCO[Si](C)(Cl)Cl AXTPGQHJFRSSQJ-UHFFFAOYSA-N 0.000 claims description 22
- 229920005610 lignin Polymers 0.000 claims description 21
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 17
- 229920001661 Chitosan Polymers 0.000 claims description 16
- 239000005543 nano-size silicon particle Substances 0.000 claims description 16
- 235000012239 silicon dioxide Nutrition 0.000 claims description 16
- 239000013464 silicone adhesive Substances 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 15
- 239000012074 organic phase Substances 0.000 claims description 15
- DFQPZDGUFQJANM-UHFFFAOYSA-M tetrabutylphosphanium;hydroxide Chemical compound [OH-].CCCC[P+](CCCC)(CCCC)CCCC DFQPZDGUFQJANM-UHFFFAOYSA-M 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 239000004945 silicone rubber Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- DEZDKWLZZLEVST-UHFFFAOYSA-N tetrabutyl(hydroxy)-$l^{5}-phosphane Chemical compound CCCCP(O)(CCCC)(CCCC)CCCC DEZDKWLZZLEVST-UHFFFAOYSA-N 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 5
- 239000010452 phosphate Substances 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 108010009736 Protein Hydrolysates Proteins 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 150000004671 saturated fatty acids Chemical class 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 11
- 230000000875 corresponding effect Effects 0.000 description 11
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 8
- 239000011148 porous material Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 238000006482 condensation reaction Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 230000003301 hydrolyzing effect Effects 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 3
- -1 polydimethylsiloxane Polymers 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 229960000892 attapulgite Drugs 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052625 palygorskite Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The application specifically discloses an organic silica gel adhesive. The organic silica gel adhesive comprises the following raw materials: 90-100 parts of 107 silicon rubber, 20-30 parts of modified white carbon black, 2-4 parts of graphene oxide, 2-5 parts of zinc stearate, 8-16 parts of modified nano calcium carbonate and 3-10 parts of dioctyl phthalate; the application also defines the preparation methods of the modified white carbon black and the modified nano calcium carbonate. The organic silica gel adhesive prepared by the application has higher mechanical strength and bonding strength, and has better performance when being subsequently applied to various fields.
Description
Technical Field
The application relates to the technical field of high polymer materials, in particular to an organic silica gel adhesive.
Background
The 107 silicone rubber is hydroxyl-terminated polydimethylsiloxane, is mixed with a catalyst and a cross-linking agent, is cured at room temperature, can keep elasticity for a long time within the temperature range of 80-200 ℃, has excellent electrical property and chemical stability, is commonly used in organic silicone adhesives, improves the comprehensive performance of the organic silicone adhesives, and has wide implementation value when the organic silicone adhesives are implemented in insulation of electronic elements, caulking of buildings and molding of rubber and plastic products.
The organic silica gel adhesive in the prior art has excellent adhesive performance and high temperature resistance, but has insufficient mechanical properties in the process of actually preparing the organic silica gel adhesive, so that the organic silica gel adhesive is cracked and even falls off in the use process, and further the implementation of the organic silica gel adhesive is limited.
Disclosure of Invention
In order to solve the problem of insufficient mechanical properties in the preparation process of the organic silica gel adhesive, the application provides the organic silica gel adhesive.
In a first aspect, the present application provides an organosilicon adhesive comprising the following raw materials: 90-100 parts of 107 silicon rubber, 20-30 parts of modified white carbon black, 2-4 parts of graphene oxide, 2-5 parts of zinc stearate, 8-16 parts of modified nano calcium carbonate and 3-10 parts of dioctyl phthalate;
the preparation method of the modified white carbon black comprises the following steps:
(1) Dispersing white carbon black in a sodium hydroxide solution, stirring for 2-3h, filtering, dispersing in deionized water again, adding nano silicon dioxide, and stirring for 1-2h at 60-64 ℃ to obtain a mixed solution;
(2) Respectively adding hydroxyethyl cellulose, lignin and a silane coupling agent into the mixed solution obtained in the step (1), stirring for 2-3 hours at the temperature of 80-85 ℃, filtering, and drying to obtain modified white carbon black;
the preparation method of the modified nano calcium carbonate comprises the following steps:
(1) Dispersing nano calcium carbonate in deionized water, adding saturated fatty acid sodium, continuously stirring for 2-3h, filtering, and drying to obtain pretreated calcium carbonate;
(2) Dispersing hydrotalcite in ammonia water, stirring for 1-2h, washing with water, filtering, grinding, sieving, calcining at 300-320 ℃ for 1-2h to obtain treated hydrotalcite;
(3) Dispersing the calcium carbonate treated in the step (1) in deionized water, adding the hydrotalcite treated in the step (2), adding citric acid and chitosan, stirring for 3-5h, filtering, and drying to obtain the modified nano calcium carbonate.
By adopting the technical scheme, the 107 silicon rubber has excellent mechanical property, high bonding strength and excellent insulativity, the modified white carbon black has higher specific surface area, strength, hardness and wear resistance, the strength, toughness and wear resistance of the system can be improved, and the graphene oxide has better flexibility, elasticity, chemical stability and mechanical property, and the strength of the system can be improved; the zinc stearate has lubricity, stability and thickening property, so that all raw material components are uniformly mixed, the modified nano calcium carbonate has a space three-dimensional structure and good dispersibility, the strength of a system can be enhanced, dioctyl phthalate has good plasticity, the flexibility and the processability of the system can be improved, the hardness and the brittleness of plastics are reduced, and the prepared organic silica gel adhesive has good mechanical properties;
the sodium hydroxide is used for carrying out certain degradation on the surface of the white carbon black, so that the organic impurities on the surface of the white carbon black are removed, the porosity of the white carbon black is improved, the specific surface area of the white carbon black is increased, the nano silicon dioxide has higher strength and can be loaded in the pores of the white carbon black, and the strength of the white carbon black is further increased.
The hydroxyethyl cellulose has good cohesiveness and heat resistance, the lignin has certain viscosity, the hydroxyethyl cellulose can play a role in lubrication, the mixing of the hydroxyethyl cellulose and the lignin can improve the lubricity and the viscosity of a system, and the silane coupling agent can be respectively crosslinked with the hydroxyethyl cellulose and the lignin to form a reticular macromolecule, so that the subsequent coating of the white carbon black is facilitated, the connection between the white carbon black and the nano silica is tighter, the performance stability of the white carbon black is further improved, the mechanical property of the white carbon black is improved, and the subsequent modification of the organic silica adhesive is facilitated.
The nano calcium carbonate is dispersed in deionized water, and the saturated fatty acid sodium has a certain dispersing effect on the nano calcium carbonate, so that the nano calcium carbonate is uniformly dispersed; the hydrotalcite has higher hardness and mechanical strength and higher impact resistance, ammonia water carries out certain degradation on the surface of the hydrotalcite, so that the surface of the hydrotalcite becomes loose and porous, and then the hydrotalcite is calcined at 300-320 ℃, so that organic impurities in the hydrotalcite are further removed, and the porosity and specific surface area of the hydrotalcite are improved.
The calcium carbonate treated in the step (1) and the hydrotalcite treated in the step (2) are mixed, the calcium carbonate is loaded in the pore structure of the hydrotalcite, so that the mechanical strength of the hydrotalcite is improved, and the surface of the hydrotalcite is coated by chitosan, so that the hydrotalcite and the calcium carbonate are combined more tightly, the performance stability of the hydrotalcite is improved, the strength stability of the hydrotalcite is improved, and the prepared modified nano calcium carbonate has better mechanical strength.
Preferably, the mass ratio of the modified white carbon black to the graphene oxide to the modified nano calcium carbonate is 8-12:1:3-5.
By adopting the technical scheme, the modified white carbon black has higher specific surface area, the modified nano calcium carbonate can be loaded in the pore structure of the modified white carbon black, the modified white carbon black can be loaded on the surface of the graphene oxide, so that the mechanical property of the modified white carbon black is improved, the modified white carbon black, the graphene oxide and the modified nano calcium carbonate are matched with each other, the mechanical property of the white carbon black is improved together, the modified white carbon black is applied to an organic silica gel adhesive subsequently, and the corresponding property of the organic silica gel adhesive is improved.
Preferably, the mass ratio of the white carbon black to the nano silicon dioxide to the hydroxyethyl cellulose is 1:0.7-0.9:0.2-0.5.
By adopting the technical scheme, the mass ratio of the white carbon black, the nano silicon dioxide and the hydroxyethyl cellulose is further limited within a certain range, so that the modified white carbon black with higher mechanical strength is obtained, the nano silicon dioxide is loaded on the surface and in the pores of the white carbon black, and the hydroxyethyl cellulose can coat the white carbon black, so that the viscosity between the white carbon black and the nano silicon dioxide is enhanced, the performance of the modified white carbon black is stable, and the corresponding performance of the white carbon black is improved.
Preferably, the mass ratio of the hydroxyethyl cellulose to the lignin to the silane coupling agent is 1:0.3-0.6:0.05-0.08.
By adopting the technical scheme, the mass ratio of the hydroxyethyl cellulose, the lignin and the silane coupling agent is further limited within a certain range, the subsequent modified white carbon black is better in performance, the silane coupling agent can be crosslinked with the hydroxyethyl cellulose and the lignin to form a network structure, the mechanical property of a system is further improved, the network structure formed by the hydroxyethyl cellulose, the lignin and the silane coupling agent has a certain coating on the white carbon black, the white carbon black and the nano silicon dioxide are bonded more stably, and the performance of the modified white carbon black is further stable.
Preferably, the mass ratio of the nano calcium carbonate to the hydrotalcite to the chitosan is 1:0.2-0.5:0.03-0.06.
By adopting the technical scheme, the mass ratio of the nano calcium carbonate, the hydrotalcite and the chitosan is further limited within a certain range, so that the modified nano calcium carbonate has better mechanical strength, the nano calcium carbonate is loaded on the surface and the pores of the hydrotalcite, and the chitosan coats the hydrotalcite and the nano calcium carbonate to a certain extent, so that the nano calcium carbonate and the hydrotalcite are more tightly connected, the performance stability and the mechanical strength of the nano calcium carbonate are further improved, and the subsequent improvement of the corresponding performance of the organic silica gel adhesive is facilitated.
Preferably, in the step (3), the stirring temperature is 60-65 ℃ and the stirring speed is 1000-1200r/min.
By adopting the technical scheme, the stirring temperature and time are further limited, so that the components are uniformly mixed, the respective functions are fully exerted, and the prepared organic silica gel adhesive has more stable comprehensive performance.
Preferably, the preparation process of the 107 silicon rubber comprises the following steps:
(1) Adding dimethyl dichlorosilane, tetrabutyl phosphorus hydroxide and methyl ethoxy dichlorosilane into a methanol solution with the mass concentration of 25-46%, stirring for 40-45min to obtain a hydrolysate, then adding potassium hydroxide, adjusting the pH value to 8-9, carrying out heat preservation reaction until the viscosity of an organic phase is 2000-2100cp, and carrying out centrifugal separation to obtain an organic phase;
(2) Adding phosphate into the organic phase, stirring uniformly, heating to 160-180 ℃ and preserving heat for 1-2h, and then removing the silicon rubber for 1-3h under vacuum of-0.05-0.101 MPa to obtain the 107 silicon rubber.
By adopting the technical scheme, the alpha, omega-dihydroxyl polydimethylsiloxane is prepared by adopting the hydrolytic condensation of the dimethyldichlorosilane, the methylethoxy dichlorosilane is added to hydrolyze the silicon-chlorine bond in the dimethyldichlorosilane into silicon hydroxyl, tetrabutyl phosphonium hydroxide is used as a catalyst, the ethoxy in the methylethoxy dichlorosilane does not participate in the hydrolysis, the ethoxy group is reserved, and in the subsequent condensation reaction process, the pH value of a reaction system is controlled to prevent the ethoxy from hydrolytic crosslinking in the condensation reaction process, so that the 107 glue crude product with ethoxy in the side chain is obtained.
And adding phosphate into the organic phase to increase the adhesive force of the organic phase, and heating at 160-180 ℃ to evaporate the solvent in the organic phase to obtain 107 silicon rubber, thereby improving the adhesive strength and the surface drying time of the 107 silicon rubber.
Preferably, the mass ratio of the dimethyl dichlorosilane to the tetrabutyl phosphonium hydroxide to the methylethoxy dichlorosilane is 10-15:1:4-5.
By adopting the technical scheme, the mass ratio of the dimethyldichlorosilane, the tetrabutyl phosphonium hydroxide and the methylethoxy dichlorosilane is further limited within a certain range, the reaction efficiency of the dimethyldichlorosilane, the tetrabutyl phosphonium hydroxide and the methylethoxy dichlorosilane is improved, the dimethyldichlorosilane is fully hydrolyzed, and the subsequently prepared 107 silicon rubber has better comprehensive performance.
In summary, the application has the following beneficial effects:
1. in the method, dimethyl dichlorosilane is adopted for hydrolytic condensation to prepare alpha, omega-dihydroxyl polydimethylsiloxane, methyl ethoxy dichlorosilane is added to hydrolyze silicon-chlorine bond in the dimethyl dichlorosilane into silicon hydroxyl, tetrabutyl phosphorus hydroxide is used as a catalyst, ethoxy in the methyl ethoxy dichlorosilane does not participate in hydrolysis, ethoxy groups are reserved, the pH value of a reaction system is controlled in the subsequent condensation reaction process, so that ethoxy hydrolysis crosslinking is prevented in the condensation reaction process, and a 107 glue crude product with ethoxy groups in side chains is obtained.
2. The mass ratio of the dimethyldichlorosilane, the tetrabutyl phosphorus hydroxide and the methylethoxy dichlorosilane is limited in a certain range, the reaction efficiency of the dimethyldichlorosilane, the tetrabutyl phosphorus hydroxide and the methylethoxy dichlorosilane is improved, the dimethyldichlorosilane is fully hydrolyzed, and the 107 silicone rubber prepared later has better comprehensive performance.
3. The 107 silicon rubber has excellent mechanical properties, high bonding strength and excellent insulativity, the modified white carbon black has higher specific surface area, strength, hardness and wear resistance, the strength, toughness and wear resistance of a system can be improved, and the graphene oxide has better flexibility, elasticity, chemical stability and mechanical properties, and the strength of the system can be improved; the modified nano calcium carbonate has a space three-dimensional structure and good dispersibility, can enhance the strength of a system, and can improve the comprehensive performance of the system together by mutually matching the components.
Detailed Description
The present application is described in further detail below with reference to examples.
The raw materials used in examples and comparative examples are all commercially available.
PREPARATION EXAMPLE 1-1
The preparation method of the modified white carbon black comprises the following steps:
(1) Dispersing 1.2kg of white carbon black in 2L of 10% sodium hydroxide solution, stirring for 2.5h, filtering, dispersing in 3L of deionized water, adding nano silicon dioxide, and stirring for 1.5h at 62 ℃ to obtain a mixed solution;
(2) And (3) respectively adding hydroxyethyl cellulose, lignin and a silane coupling agent into the mixed solution obtained in the step (1), stirring for 2.5 hours at the temperature of 82 ℃, filtering, and drying to obtain the modified white carbon black.
The mass ratio of the white carbon black to the nano silicon dioxide to the hydroxyethyl cellulose is 1:0.7:0.5.
The mass ratio of the hydroxyethyl cellulose to the lignin to the silane coupling agent is 1:0.3:0.05.
PREPARATION EXAMPLES 1-2
The difference from preparation example 1-1 is that no nanosilica was added in step (1).
Preparation examples 1 to 3
The difference from preparation example 1-1 is that in step (2), hydroxyethylcellulose is not added.
Preparation examples 1 to 4
The difference from preparation example 1-1 is that lignin is not added in step (2).
Preparation examples 1 to 5
The difference from preparation example 1-1 is that in step (2), a silane coupling agent is not added.
Preparation examples 1 to 6
The difference from preparation example 1-1 is that the mass ratio of white carbon black, nano silicon dioxide and hydroxyethyl cellulose is 1:0.9:0.2.
The mass ratio of the hydroxyethyl cellulose to the lignin to the silane coupling agent is 1:0.6:0.08.
Preparation examples 1 to 7
The difference from preparation example 1-1 is that the mass ratio of white carbon black, nano silicon dioxide and hydroxyethyl cellulose is 1:0.3:0.9.
Preparation examples 1 to 8
The difference from preparation example 1-1 is that the mass ratio of hydroxyethyl cellulose, lignin and silane coupling agent is 1:0.1:0.3.
PREPARATION EXAMPLE 2-1
The preparation method of the modified nano calcium carbonate comprises the following steps:
(1) Dispersing 0.8kg of nano calcium carbonate in 2L of deionized water, adding 0.2kg of saturated fatty acid sodium, continuously stirring for 2.5h, filtering, and drying to obtain pretreated calcium carbonate;
(2) Dispersing hydrotalcite in 2L of 5% de ammonia water, stirring for 1.5h, washing with water, filtering, grinding, sieving with a 20-mesh sieve, and calcining at 310 ℃ for 1.5h to obtain treated hydrotalcite;
(3) Dispersing the calcium carbonate treated in the step (1) in 2L of deionized water, adding the hydrotalcite treated in the step (2), adding 0.3kg of citric acid and chitosan, stirring for 4 hours, filtering and drying to obtain the modified nano calcium carbonate.
The mass ratio of the nano calcium carbonate to the hydrotalcite to the chitosan is 1:0.5:0.03.
In the step (3), the stirring temperature was 60℃and the stirring rate was 1000r/min.
PREPARATION EXAMPLE 2-2
The difference from preparation example 2-1 is that hydrotalcite was not added in step (2).
PREPARATION EXAMPLES 2-3
The difference from preparation example 2-1 is that chitosan was not added in step (3).
PREPARATION EXAMPLES 2 to 4
The difference from preparation example 2-1 is that the mass ratio of nano calcium carbonate, hydrotalcite and chitosan is 1:0.2:0.06.
In the step (3), the stirring temperature was 65℃and the stirring rate was 1200r/min.
PREPARATION EXAMPLES 2 to 5
The difference from preparation example 2-1 is that the mass ratio of nano calcium carbonate, hydrotalcite and chitosan is 1:0.1:0.2.
Example 1
An organic silica gel adhesive comprises the following raw materials: 100kg of 107 silicone rubber, 20kg of modified white carbon black, 4kg of graphene oxide, 5kg of zinc stearate, 16kg of modified nano calcium carbonate and 10kg of dioctyl phthalate.
Preparation example 1-1 is adopted for the modified white carbon black, and preparation example 2-1 is adopted for the modified nano calcium carbonate.
The preparation process of the 107 silicon rubber comprises the following steps:
(1) Adding dimethyl dichlorosilane, 1kg of tetrabutyl phosphorus hydroxide and methyl ethoxy dichlorosilane into a methanol solution with the mass concentration of 25%, stirring for 40min to obtain a hydrolysate, then adding 30% potassium hydroxide, adjusting the pH value to 9, carrying out heat preservation reaction until the viscosity of an organic phase is 2000cp, and carrying out centrifugal separation to obtain an organic phase;
(2) Adding 0.4kg of phosphate into the organic phase, stirring uniformly, heating to 180 ℃, preserving heat for 1-2h, and removing the solution for 1h under the vacuum of-0.05 MPa to obtain the 107 silicone rubber.
The mass ratio of the dimethyldichlorosilane to the tetrabutyl phosphonium hydroxide to the methylethoxy dichlorosilane is 10:1:5.
Example 2
The silicone adhesive differs from example 1 in that the preparation process of 107 silicone rubber comprises the following steps: (1) Adding dimethyl dichlorosilane, tetrabutyl phosphorus hydroxide and methyl ethoxy dichlorosilane into a methanol solution with the mass concentration of 46%, stirring for 45min to obtain a hydrolysate, then adding 30% potassium hydroxide with the mass fraction, adjusting the pH value to 8, carrying out heat preservation reaction until the viscosity of an organic phase is 2100cp, and carrying out centrifugal separation to obtain an organic phase;
(2) Adding 0.3kg of phosphate into the organic phase, stirring uniformly, heating to 160 ℃, preserving heat for 1-2h, and removing the solution for 3h under the vacuum of-0.101 MPa to obtain the 107 silicone rubber.
The mass ratio of the dimethyldichlorosilane to the tetrabutyl phosphonium hydroxide to the methylethoxy dichlorosilane is 15:1:4.
Example 3
The silicone adhesive differs from example 1 in that the mass ratio of dimethyldichlorosilane, tetrabutylphosphonium hydroxide and methylethoxydichloride silane is 18:1:2.
Example 4
The silicone adhesive differs from example 1 in that it comprises the following raw materials: 90kg of 107 silicone rubber, 30kg of modified white carbon black, 2kg of graphene oxide, 2kg of zinc stearate, 8kg of modified nano calcium carbonate and 3kg of dioctyl phthalate.
Example 5
An organic silica gel adhesive is different from example 1 in that the modified white carbon black is prepared in preparation examples 1-2.
Example 6
An organic silica gel adhesive differs from example 1 in that modified white carbon black was used in preparation examples 1 to 3.
Example 7
An organic silica gel adhesive differs from example 1 in that modified white carbon black was used in preparation examples 1 to 4.
Example 8
An organic silica gel adhesive differs from example 1 in that modified white carbon black was used in preparation examples 1 to 5.
Example 9
An organic silica gel adhesive differs from example 1 in that modified white carbon black was used in preparation examples 1 to 6.
Example 10
An organic silica gel adhesive differs from example 1 in that modified white carbon black was used in preparation examples 1 to 7.
Example 11
An organic silica gel adhesive differs from example 1 in that modified white carbon black was used in preparation examples 1 to 8.
Example 12
An organic silica gel adhesive is different from example 1 in that the modified nano calcium carbonate is prepared in preparation examples 2-2.
Example 13
An organic silica gel adhesive is different from example 1 in that the modified nano calcium carbonate was used in preparation examples 2 to 3.
Example 14
An organic silica gel adhesive is different from example 1 in that the modified nano calcium carbonate was used in preparation examples 2 to 4.
Example 15
The silicone adhesive differs from example 1 in that modified nano calcium carbonate was used in preparation examples 2-5.
Example 16
The organic silica gel adhesive is different from the embodiment 1 in that the mass ratio of the modified white carbon black to the graphene oxide to the modified nano calcium carbonate is 8:1:5.
Example 17
The organic silica gel adhesive is different from the embodiment 1 in that the mass ratio of the modified white carbon black to the graphene oxide to the modified nano calcium carbonate is 12:1:3.
Comparative example 1
An organic silica gel adhesive is different from example 1 in that modified white carbon black is not added.
Comparative example 2
An organic silica gel adhesive differs from example 1 in that the same amount of modified white carbon black is replaced with white carbon black.
Comparative example 3
An organic silica gel adhesive is different from example 1 in that graphene oxide is not added.
Comparative example 4
An organic silica gel adhesive is different from example 1 in that modified nano calcium carbonate is not added.
Comparative example 5
An organic silica gel adhesive differs from example 1 in that an equivalent amount of nano calcium carbonate is used instead of modified nano calcium carbonate.
The silicone adhesives prepared in examples 1 to 17 and comparative examples 1 to 5 were subjected to the following performance tests;
tensile strength and elongation at break were tested according to GB/T528-2009, and tear strength was tested according to ASTMD 624;
the silicone adhesive prepared in the application example and the comparative example was subjected to pressure reduction to remove bubbles, then coated on glass plates with a length of 8cm, a width of 4cm and a thickness of 2mm, respectively, with a thickness of 0.6mm, and the other glass plates with the same size were overlapped, then heated to 55 ℃ for 25min, taken out, cooled to room temperature and cured, and tested by a tensile machine, and the test results are shown in table 1.
Table 1 test data for examples and comparative examples
As can be seen from Table 1, the silicone adhesives prepared in examples 1-2, 4, 9 and 14 of the present application have better mechanical strength and mechanical strength, wherein the tensile strength of example 1 is 4.6MPa, the elongation at break is 452%, the tear strength is 62N/mm, and the bonding strength is 48N/cm, which indicates that the 107 silicone rubber prepared in the present application has better strength, and the silicone adhesive has better mechanical properties, and the components in the present application are mutually matched, so that the prepared silicone adhesive is widely implemented.
In the preparation process of 107 silicon rubber in example 3, the mass ratio of dimethyl dichlorosilane, tetrabutyl phosphonium hydroxide and methylethoxy dichlorosilane is changed, and compared with example 1, the preparation process has the advantages that the tensile strength is 4.0MPa, the elongation at break is 442%, the tearing strength is 53N/mm, the bonding strength is 38N/cm, the matching of the dimethyl dichlorosilane, the tetrabutyl phosphonium hydroxide and the methylethoxy dichlorosilane has better performance, the mass ratio of the dimethyl dichlorosilane, the tetrabutyl phosphonium hydroxide and the methylethoxy dichlorosilane is in a certain range, the reaction efficiency of the dimethyl dichlorosilane, the tetrabutyl phosphonium hydroxide and the methylethoxy dichlorosilane is improved, the dimethyl dichlorosilane is fully hydrolyzed, and the 107 silicon rubber prepared later has better comprehensive performance.
As can be seen from Table 1, compared with example 1, the preparation method of the modified white carbon black of example 5 does not add nano silicon dioxide, and has tensile strength of 3.5MPa, elongation at break of 431%, tear strength of 45N/mm and bonding strength of 32N/cm, which indicates that the nano silicon dioxide has higher strength and can be loaded in the pores of the white carbon black, thereby increasing the strength of the white carbon black.
As can be seen from Table 1, compared with example 1, the modified white carbon black of example 6 has a tensile strength of 3.7MPa, an elongation at break of 435%, a tear strength of 48N/mm and a bonding strength of 34N/cm, and the modified white carbon black of example 6 has good bonding property and heat resistance, and can be used for coating the white carbon black, thereby improving the corresponding performance of the white carbon black.
As can be seen from Table 1, compared with example 1, the modified white carbon black of example 7 has tensile strength of 3.8MPa, elongation at break of 437%, tear strength of 50N/mm and bonding strength of 33N/cm, which shows that lignin has a certain viscosity, and the mixing of hydroxyethyl cellulose and lignin can improve the lubricity and viscosity of the system, further coat the white carbon black and improve the corresponding performance of the white carbon black.
As can be seen from Table 1, compared with example 1, the preparation method of the modified white carbon black has tensile strength of 3.9MPa, elongation at break of 440%, tear strength of 51N/mm and bonding strength of 36N/cm, and the silane coupling agent can be crosslinked with hydroxyethyl cellulose and lignin respectively to form a network-structured macromolecule, so that the subsequent coating of the white carbon black is facilitated, and the corresponding performance of the white carbon black is improved.
In example 10, the mass ratio of the white carbon black, the nano silica and the hydroxyethyl cellulose is changed, and compared with example 1, the tensile strength, the elongation at break, the tearing strength and the bonding strength are all larger than those of examples 5-7, but are worse than those of examples 1 and 9, which shows that the nano silica is loaded on the surface and in the pores of the white carbon black, and the hydroxyethyl cellulose can coat the white carbon black, so that the viscosity between the white carbon black and the nano silica is enhanced, the performance of the modified white carbon black is stable, and the corresponding performance of the white carbon black is improved.
In example 11, the mass ratio of hydroxyethyl cellulose, lignin and a silane coupling agent is changed, and compared with example 1, the tensile strength, the elongation at break, the tearing strength and the bonding strength are all larger than those of examples 6-8, but are worse than example 1, which shows that the silane coupling agent can be crosslinked with the hydroxyethyl cellulose and lignin to form a network structure, so that the mechanical property of the system is improved, and the network structure formed by the hydroxyethyl cellulose, lignin and the silane coupling agent subsequently has a certain coating on the white carbon black, so that the white carbon black and nano silicon dioxide are bonded more stably, and the performance of the modified white carbon black is further stable.
In the preparation method of the modified nano calcium carbonate of example 12, hydrotalcite is not added, and compared with example 1, the preparation method has the advantages of 3.2MPa of tensile strength, 425% of elongation at break, 40N/mm of tear strength and 28N/cm of bonding strength, and shows that the hydrotalcite has higher hardness and mechanical strength, has higher impact resistance and is beneficial to subsequent improvement of the corresponding performance of the nano calcium carbonate.
In the preparation method of the modified nano calcium carbonate of example 13, no chitosan is added, and compared with example 1, the tensile strength is 3.5MPa, the elongation at break is 430%, the tearing strength is 44N/mm, and the bonding strength is 30N/cm, which shows that the chitosan coats the surface of hydrotalcite, so that the hydrotalcite and the calcium carbonate are combined more tightly, the performance stability of the hydrotalcite is further improved, the strength stability of the hydrotalcite is improved, and the prepared modified nano calcium carbonate has better mechanical strength.
In example 15, the mass ratio of attapulgite, nano calcium carbonate, hydrotalcite and chitosan is changed, and it can be seen from table 1 that, compared with example 1, the tensile strength, elongation at break, tear strength and bonding strength are all greater than those of examples 12-13, but are inferior to those of examples 1 and 14, which shows that nano calcium carbonate is loaded on the surface and in the pores of hydrotalcite, and chitosan coats hydrotalcite and nano calcium carbonate to a certain extent, so that nano calcium carbonate and hydrotalcite are more tightly connected, and further, the performance stability and mechanical strength of nano calcium carbonate are improved, and the subsequent improvement of the corresponding performance of the organic silica gel adhesive is facilitated.
Examples 16-17 change the mass ratio of the modified white carbon black, the graphene oxide and the modified nano calcium carbonate, and as can be seen from table 1, compared with example 1, the tensile strength, the elongation at break, the tearing strength and the bonding strength are all larger than those of example 1-2, which shows that the mass ratio of the dimethyl dichlorosilane, the tetrabutyl phosphonium hydroxide and the methylethoxy dichlorosilane is in a certain range, the reaction efficiency of the dimethyl dichlorosilane, the tetrabutyl phosphonium hydroxide and the methylethoxy dichlorosilane is improved, the dimethyl dichlorosilane is fully hydrolyzed, and the 107 silicon rubber prepared later has better comprehensive performance.
As can be seen from Table 1, compared with example 1, the tensile strength is 2.2MPa, the elongation at break is 400%, the tearing strength is 29N/mm, and the bonding strength is 20N/cm, and the modified white carbon black has higher specific surface area, strength, hardness and wear resistance and can improve the strength, toughness and wear resistance of the system.
As can be seen from Table 1, compared with example 1, the modified white carbon black of comparative example 2, in which the equivalent amount of the modified white carbon black is replaced by white carbon black, the tensile strength is 2.5MPa, the elongation at break is 410%, the tear strength is 32N/mm, and the bonding strength is 23N/cm, the modified white carbon black prepared by the method has better mechanical properties, and the corresponding properties of the adhesive are improved when the modified white carbon black is subsequently applied to the organic silica gel adhesive.
As can be seen from Table 1, compared with example 1, the tensile strength is 2.4MPa, the elongation at break is 409%, the tearing strength is 31N/mm, and the bonding strength is 22N/cm, which indicates that the graphene oxide has good flexibility, elasticity, chemical stability and mechanical properties, can improve the strength of the system, and is beneficial to improving the comprehensive properties of the system.
Compared with the embodiment 1, the tensile strength is 2.0MPa, the breaking elongation is 394%, the tearing strength is 27N/mm, and the bonding strength is 18N/cm, as can be seen from Table 1, the modified nano calcium carbonate prepared by the method has a spatial three-dimensional structure and good dispersibility, the strength of a system can be enhanced, and the corresponding performance of the organic silica gel adhesive is improved subsequently.
The comparative example 5 is implemented by replacing the modified nano calcium carbonate with the nano calcium carbonate with equivalent amount, and compared with the example 1, the tensile strength is 2.3MPa, the elongation at break is 398%, the tearing strength is 30N/mm, and the bonding strength is 21N/cm, so that the modified nano calcium carbonate prepared by the application has better performance, is implemented in the organic silica gel adhesive subsequently, and improves the mechanical property of the organic silica gel adhesive.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (8)
1. The organic silica gel adhesive is characterized by comprising the following raw materials: 90-100 parts of 107 silicon rubber, 20-30 parts of modified white carbon black, 2-4 parts of graphene oxide, 2-5 parts of zinc stearate, 8-16 parts of modified nano calcium carbonate and 3-10 parts of dioctyl phthalate;
the preparation method of the modified white carbon black comprises the following steps:
(1) Dispersing white carbon black in a sodium hydroxide solution, stirring for 2-3h, filtering, dispersing in deionized water again, adding nano silicon dioxide, and stirring for 1-2h at 60-64 ℃ to obtain a mixed solution;
(2) Respectively adding hydroxyethyl cellulose, lignin and a silane coupling agent into the mixed solution obtained in the step (1), stirring for 2-3 hours at the temperature of 80-85 ℃, filtering, and drying to obtain modified white carbon black;
the preparation method of the modified nano calcium carbonate comprises the following steps:
(1) Dispersing nano calcium carbonate in deionized water, adding saturated fatty acid sodium, continuously stirring for 2-3h, filtering, and drying to obtain pretreated calcium carbonate;
(2) Dispersing hydrotalcite in ammonia water, stirring for 1-2h, washing with water, filtering, grinding, sieving, calcining at 300-320 ℃ for 1-2h to obtain treated hydrotalcite;
(3) Dispersing the calcium carbonate treated in the step (1) in deionized water, adding the hydrotalcite treated in the step (2), adding citric acid and chitosan, stirring for 3-5h, filtering, and drying to obtain the modified nano calcium carbonate.
2. The organic silica gel adhesive according to claim 1, wherein the mass ratio of the modified white carbon black to the graphene oxide to the modified nano calcium carbonate is 8-12:1:3-5.
3. The organic silica gel adhesive according to claim 1, wherein the mass ratio of the white carbon black, the nano silicon dioxide and the hydroxyethyl cellulose is 1:0.7-0.9:0.2-0.5.
4. The silicone adhesive of claim 1, wherein the mass ratio of hydroxyethyl cellulose, lignin and silane coupling agent is 1:0.3-0.6:0.05-0.08.
5. The organic silica gel adhesive according to claim 1, wherein the mass ratio of the nano calcium carbonate to the hydrotalcite to the chitosan is 1:0.2-0.5:0.03-0.06.
6. The silicone adhesive of claim 1, wherein in step (3), the temperature of stirring is 60-65 ℃ and the stirring rate is 1000-1200r/min.
7. The silicone adhesive according to claim 1, wherein the process for preparing 107 silicone rubber comprises the steps of:
(1) Adding dimethyl dichlorosilane, tetrabutyl phosphorus hydroxide and methyl ethoxy dichlorosilane into a methanol solution with the mass concentration of 25-46%, stirring for 40-45min to obtain a hydrolysate, then adding potassium hydroxide, adjusting the pH value to 8-9, carrying out heat preservation reaction until the viscosity of an organic phase is 2000-2100cp, and carrying out centrifugal separation to obtain an organic phase;
(2) Adding phosphate into the organic phase, stirring uniformly, heating to 160-180 ℃ and preserving heat for 1-2h, and then removing the silicon rubber for 1-3h under vacuum of-0.05-0.101 MPa to obtain the 107 silicon rubber.
8. The silicone adhesive of claim 7, wherein the mass ratio of dimethyl dichlorosilane, tetrabutyl phosphonium hydroxide and methylethoxy dichlorosilane is 10-15:1:4-5.
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