CN111139027A - Organic silicon pressure-sensitive adhesive-based adhesive and preparation method thereof - Google Patents
Organic silicon pressure-sensitive adhesive-based adhesive and preparation method thereof Download PDFInfo
- Publication number
- CN111139027A CN111139027A CN202010026035.8A CN202010026035A CN111139027A CN 111139027 A CN111139027 A CN 111139027A CN 202010026035 A CN202010026035 A CN 202010026035A CN 111139027 A CN111139027 A CN 111139027A
- Authority
- CN
- China
- Prior art keywords
- sensitive adhesive
- pressure
- silicone
- adhesive
- preparing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- C09J183/10—Block or graft copolymers containing polysiloxane sequences
-
- 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
- C08G77/02—Polysilicates
-
- 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
-
- 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
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
-
- 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
- C08G77/70—Siloxanes defined by use of the MDTQ nomenclature
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Silicon Polymers (AREA)
Abstract
The invention discloses an organic silicon pressure-sensitive adhesive base adhesive which is composed of MQ silicon resin polycondensate and vinyl silicone oil, and has the characteristics of difficult solvent residue, safety and environmental protection, and proper bonding strength of prepared organic silicon pressure-sensitive adhesive products. The invention also provides a preparation method of the organic silicon pressure-sensitive adhesive base adhesive, which specifically comprises two steps of preparing the MQ silicon resin prepolymer solution and carrying out reduced pressure polycondensation with the vinyl silicone oil at the temperature of 180 ℃ with the addition of 120-.
Description
Technical Field
The invention relates to the technical field of organic silicon materials, in particular to an organic silicon pressure-sensitive adhesive base adhesive and a preparation method thereof.
Background
Pressure Sensitive Adhesives (PSAs) are a class of adhesives that are sensitive to pressure. The organosilicon pressure-sensitive adhesive is a high-quality pressure-sensitive adhesive with wide application, generally takes Si-O bond as a main chain, takes an organic group as a side chain, has the characteristics of organic materials and inorganic materials, can keep stable physical and chemical properties in a wider condition range, has good high and low temperature resistance, chemical inertness, water resistance, weather resistance, corrosion resistance, acid and alkali resistance, liquid permeability, biological inertness, flexibility and shock absorption, can be bonded with materials with low surface energy, even can be bonded with interfaces with moisture and oil, and is widely applied to the fields of industry, electronics, medical use and the like.
At present, the organic silicon pressure-sensitive adhesives on the market can be divided into two main categories according to a vulcanization system: peroxide vulcanization type developed in the 70 th of the 20 th century is prepared by performing catalytic polycondensation on hydroxyl silicone oil and MQ silicone resin; the other type is addition type developed in the 80 th of the 20 th century, and is obtained by performing platinum-catalyzed addition on vinyl silicone oil, hydrogen-containing silicone oil and MQ silicone resin. In both vulcanization systems, MQ silicone resins are inevitably used, which can play a role in improving pressure-sensitive adhesive properties, providing tack and hold-tack, and adjusting the physical properties of the pressure-sensitive adhesive in silicone pressure-sensitive adhesives.
The prior MQ silicon resin is generally prepared by adopting a water glass and silicate method (see U.S. Pat. Nos. 2676182, 3627851, 3772247 and the like), and then the prepared MQ silicon resin is added into silicon rubber to react to prepare the organic silicon pressure-sensitive adhesive (see peroxide type organic silicon pressure-sensitive adhesive patents CN 102051154A, CN 107227143A, 5602214 and the like; addition type organic silicon pressure-sensitive adhesive patents CN 106833502A, CN 104152104B, US 5366809 and the like).
The preparation of MQ silicone resins described in the above patents has general disadvantages: the acid water is discharged in large quantity, the environment is polluted, the related process flows of extraction, water washing, solvent removal and the like are complicated, the energy consumption is high, the prepared MQ silicon resin is generally in a solid state, and the MQ silicon resin is difficult to take out of a kettle or easily causes dust pollution; in addition, MQ silicone resins prepared tend to have gels or high molecular weight polycondensates,the compatibility with silicon rubber is poor, and the turbidity of the appearance of the formula of the organic silicon pressure-sensitive adhesive is easily caused, even the organic silicon pressure-sensitive adhesive is separated out from the formula; there are also low molecular polycondensates, such as MQ silicone resins prepared according to the Daudt patent US 2676182, which contain by-products (R)3SiO)4Si, the presence of these substances tends to affect the performance of silicone pressure sensitive adhesives. When the MQ silicon resin is mixed with the silicon rubber to prepare the base sizing material of the organic silicon pressure-sensitive adhesive, the peroxide vulcanization type and addition type patents both relate to the process of firstly dissolving solid MQ powder by using an organic solvent and then mixing the solid MQ powder with the silicon rubber, and the solvent is greatly and repeatedly used in the synthesis of the MQ silicon resin and the preparation of the organic silicon pressure-sensitive adhesive, so that the cost is inevitably increased and the environment is inevitably polluted.
CN 1015906810B and CN 107226907B describe an alternative strategy for MQ silicone resin synthesis, where the preparation of MQ silicone resins using transesterification reactions avoids gelation of the product and has enhanced environmental properties.
At present, most of organic silicon pressure-sensitive adhesive base materials on the market are prepared by dissolving MQ silicon resin powder in a solvent and then mixing the dissolved MQ silicon resin powder with vinyl silicone oil, and the molecular weight of the MQ silicon resin is too large due to the fact that the rate of the MQ silicon resin prepolymer in polycondensation into the MQ silicon resin powder is difficult to control, so that the MQ silicon resin has poor compatibility with the vinyl silicone oil.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of an organic silicon pressure-sensitive adhesive base adhesive which contains less residual solvent, is safe and environment-friendly and has stable bonding performance.
The second purpose of the invention is to provide the organic silicon pressure-sensitive adhesive obtained by the preparation method of the organic silicon pressure-sensitive adhesive base adhesive.
One of the purposes of the invention is realized by adopting the following technical scheme:
a preparation method of an organic silicon pressure-sensitive adhesive base adhesive comprises the following steps:
1) preparing MQ silicon resin prepolymer solution;
2) and (3) reduced pressure polycondensation: adding vinyl silicone oil into the MQ silicone resin prepolymer solution in the step 1), heating, and carrying out reduced pressure polycondensation at the temperature of 120 ℃ and 180 ℃ for 1-6h to obtain the organic silicon pressure-sensitive adhesive base adhesive.
Further, in the step 1), the preparation of the MQ silicone resin prepolymer solution specifically comprises the following steps: mixing polysilicate, hexamethyldisiloxane, glacial acetic acid and concentrated sulfuric acid at room temperature for 0.5-2h, heating to reflux for 3-6h, cooling, adjusting pH, and layering, wherein the organic phase is MQ silicon resin prepolymer solution.
Further, in the step 1), the mol ratio of the hexamethyldisiloxane to the polysilicate to the glacial acetic acid is 0.3-0.6: 1: 2.0 to 2.4, and the using amount of concentrated sulfuric acid is 1.0 to 3.0 percent of the total mass of hexamethyldisiloxane and polysilicate. More preferably, the molar ratio of hexamethyldisiloxane to polysilicate to glacial acetic acid is 0.4: 1: 2.1. the using amount of the concentrated sulfuric acid is 2.0 percent of the total mass of the hexamethyldisiloxane and the polysilicate. The concentration of concentrated sulfuric acid is preferably 98%.
Further, in the step 1), the polysilicate is polyethyl silicate and SiO is used2The mass fraction is 30-50%.
Further, in step 1), the pH is adjusted to 7 to 9. Specifically, saturated aqueous sodium carbonate solution was used to adjust the pH to 7-9.
Further, in the step 2), the mass ratio of the MQ silicon resin prepolymer to the vinyl silicone oil is 1: 0.5-10. Preferably 1: 0.5-2. The MQ silicone prepolymer is calculated as the solids content of the MQ silicone prepolymer solution.
Further, the vinyl silicone oil is terminal vinyl polydimethylsiloxane, the viscosity of the vinyl silicone oil is in the range of 2000-50000 mPa.s, and the vinyl content of the vinyl silicone oil is 0.08-0.25%. Preferably 5000-20000 mPas and a vinyl content of 0.08-0.12%.
Further, in the step 2), the polycondensation is carried out for 1-3h at 150-160 ℃. Preferably at 150 ℃ and 155 ℃ for 1.5 h.
Further, in the step 2), the pressure reduction polycondensation is carried out until the viscosity of the organic silicon pressure-sensitive adhesive base adhesive is 5000-1000000mPa & s and the vinyl mass fraction is 0.03-0.24%. Preferably, the pressure-reducing polycondensation is carried out until the viscosity of the organic silicon pressure-sensitive adhesive base adhesive is 100000-500000 mPas and the vinyl mass fraction is 0.05-0.12%.
The second purpose of the invention is realized by adopting the following technical scheme:
the organic silicon pressure-sensitive adhesive base adhesive is prepared by the preparation method of the organic silicon pressure-sensitive adhesive base adhesive.
Compared with the prior art, the invention has the beneficial effects that:
according to the organic silicon pressure-sensitive adhesive base adhesive provided by the invention, the MQ prepolymer has relatively stable low molecular weight and relatively large amount of silicon hydroxyl reserved, and can be subjected to polycondensation under vinyl silicone oil to prepare a high-transparency gel-free organic silicon pressure-sensitive adhesive base adhesive; compared with the organic silicon pressure-sensitive adhesive base adhesive prepared by dissolving the MQ silicon resin powder which is conventionally adopted at present, the organic silicon pressure-sensitive adhesive base adhesive has better system compatibility and adhesion with a base material, and the reaction process and the polycondensation rate are more controllable, so that the organic silicon pressure-sensitive adhesive base adhesive has more stable adhesive property when applied to an organic silicon pressure-sensitive adhesive formula.
The preparation method of the organic silicon pressure-sensitive adhesive-based adhesive provided by the invention can effectively simplify the process flow, shorten the production period, avoid the use of a large amount of solvents, and has the advantages of low cost and energy consumption, environmental protection and safety; has obvious effects of improving the product yield, improving the system compatibility of MQ silicon resin and the stability of the organic silicon pressure-sensitive adhesive.
Detailed Description
The present invention is further described below with reference to specific embodiments, and it should be noted that, without conflict, any combination between the embodiments or technical features described below may form a new embodiment.
The following are specific examples of the present invention, and raw materials, equipments and the like used in the following examples can be obtained by purchasing them unless otherwise specified.
Examples 1 to 4:
225 g of SiO were placed in a 1L four-necked flask equipped with a vigorous stirring, thermometer and reflux tube240 percent of ethyl polysilicate, 97.2 grams of hexamethyldisiloxane and 198 grams of glacial acetic acid are added after being evenly stirred, 4.93 grams of 98 percent concentrated sulfuric acid is added after being stirred for 60min at normal temperature, the mixture is heated and heated, the mixture reacts for 4 hours at the reflux temperature of 76 to 78 ℃, the heating is stopped, the reaction solution is added after being cooled to the room temperature148 g of saturated aqueous sodium carbonate solution were adjusted to pH 8.5 and left to layer, giving 436.85 g of MQ silicone prepolymer solution with a solids content of 44.11%.
Adding 100 g of the MQ silicon resin prepolymer solution into 44.11 g of vinyl silicone oil (shown in Table 1) with different viscosities, uniformly stirring, heating, raising the temperature, starting a vacuum pump to pull down when the temperature reaches 150 ℃, carrying out reduced pressure polycondensation reaction at 155 ℃ for 1.5h, stopping heating, filtering while hot to obtain the organic silicon pressure-sensitive adhesive base adhesive, and obtaining product characterization results shown in Table 2.
TABLE 1 vinyl Silicone oils of different viscosities as used in examples 1-4
| Examples | Name of vinyl Silicone oil | Viscosity, mPas | Mass fraction of vinyl groups,% |
| 1 | Double-end vinyl silicone oil | 20000 | 0.10 |
| 2 | Double-end vinyl silicone oil | 10000 | 0.13 |
| 3 | Double-end vinyl silicone oil | 5000 | 0.17 |
| 4 | Double-end vinyl silicone oil | 2000 | 0.24 |
TABLE 2 characterization results of silicone pressure sensitive adhesive-based adhesives
From the data in table 2, it can be found that: the preparation method provided by the invention is suitable for preparing vinyl silicone oil mixed liquor of MQ silicone resin with different viscosities or different vinyl contents, namely the organic silicon pressure-sensitive adhesive base glue, and the prepared base glue is colorless transparent viscous liquid without generating gel substances or insoluble substances.
Examples 5 to 8
225 g of SiO were placed in a 1L four-necked flask equipped with a vigorous stirring, thermometer and reflux tube240 percent of ethyl polysilicate, 121.5 grams of hexamethyldisiloxane and 189 grams of glacial acetic acid are added after being uniformly stirred, 3.47 grams of 98 percent concentrated sulfuric acid is added, the mixture is stirred for 60min at normal temperature and then heated, the mixture is reacted for 4h at the reflux temperature of 76-78 ℃, heating is stopped, four 150 grams of reaction liquid are taken out after being cooled to the room temperature, saturated sodium carbonate aqueous solution is respectively added to adjust the pH value to be 5, 7, 8 and 9, and the mixture is kept stand and layered to obtain the MQ silicon resin prepolymer solution, wherein the solid content is 46.58 percent, 45.82 percent, 44.31 percent and 43.56 percent respectively.
And (3) respectively adding 46.58 g, 45.82 g, 44.31 g and 43.56g of double-end vinyl silicone oil with the viscosity of 20000mPa · s and the vinyl content of 0.087% into 100 g of the MQ silicon resin prepolymer solution, uniformly stirring, heating, raising the temperature, starting a vacuum pump to pull down when the temperature reaches 150 ℃, carrying out reduced pressure polycondensation reaction at 155 ℃ for 1.5h, stopping heating, filtering while hot to obtain the organic silicon pressure-sensitive adhesive base adhesive, wherein the product characterization results are listed in Table 3.
TABLE 3 characterization results of the products prepared from MQ silicone prepolymer solution
| Examples | pH of MQ prepolymer solution | Viscosity, mPas | Mass fraction of vinyl groups,% |
| 5 | 5 | 280000 | 0.0376 |
| 6 | 7 | 150000 | 0.0426 |
| 7 | 8 | 345000 | 0.0409 |
| 8 | 9 | 525000 | 0.0405 |
From the data in table 3, it can be found that: the preparation method provided by the invention is more suitable for adopting MQ silicon resin prepolymer solution with alkalescent pH, because under alkalescence, MQ silicon resin prepolymer is easier to be condensed to form MQ silicon resin with larger molecular weight; under acidic conditions, the MQ silicon resin prepolymer solution is easy to cause the reduction of the vinyl content, and in addition, the prepared organic silicon pressure-sensitive adhesive base adhesive has obvious pungent sour taste.
Examples 9 to 12
225 g of SiO were placed in a 1L four-necked flask equipped with a vigorous stirring, thermometer and reflux tube2Ethyl polysilicate with the content of 40%, 97.2 g of hexamethyldisiloxane and 198 g of glacial acetic acid are added after being stirred uniformly, 4.93 g of 98% concentrated sulfuric acid is added, the mixture is stirred for 60min at normal temperature and then heated, the reaction is carried out for 4h at the reflux temperature of 76-78 ℃, the heating is stopped, 148 g of saturated sodium carbonate aqueous solution is added after the reaction liquid is cooled to the room temperature, the pH value is adjusted to 8.5, the mixture is kept stand and layered, 436.85 g of MQ silicon resin prepolymer solution is obtained, and the solid content is 44.11%.
And adding 100 g of the MQ silicon resin prepolymer solution into 44.11 g of vinyl silicone oil with the viscosity of 20000 mPas, uniformly stirring, heating, performing reduced-pressure polycondensation reaction for 1.5h when the temperature reaches 120, 150, 160 and 180 ℃, stopping heating, and filtering while hot to obtain the organic silicon pressure-sensitive adhesive base adhesive of the embodiment 9-12.
TABLE 4 characterization results of the polycondensation temperature of the silicone pressure-sensitive adhesive-based adhesives
| Examples | Polycondensation temperature of DEG C | Viscosity, mPas | Mass fraction of vinyl groups,% |
| 9 | 120 | 186000 | 0.0512 |
| 10 | 150 | 365000 | 0.0495 |
| 11 | 160 | 425000 | 0.0486 |
| 12 | 180 | 638000 | 0.0489 |
From the above table, it can be known that the viscosity of the silicone pressure-sensitive adhesive base adhesive can be effectively improved by prolonging the polycondensation time of the MQ silicone resin or increasing the polycondensation temperature of the MQ silicone resin prepolymer and the vinyl silicone oil.
Comparative example 1:
225 g of SiO were placed in a 1L four-necked flask equipped with a vigorous stirring, thermometer and reflux tube2Ethyl polysilicate with the content of 40%, 97.2 g of hexamethyldisiloxane and 198 g of glacial acetic acid are added after being stirred uniformly, 4.93 g of 98% concentrated sulfuric acid is added, the mixture is stirred for 60min at normal temperature and then heated, the reaction is carried out for 4h at the reflux temperature of 76-78 ℃, the heating is stopped, 148 g of saturated sodium carbonate aqueous solution is added after the reaction liquid is cooled to the room temperature, the pH value is adjusted to 8.5, the mixture is kept stand and layered, 436.85 g of MQ silicon resin prepolymer is obtained, and the solid content is 44.11%.
Adding 200 g of the mixture into a 1L reaction bottle, heating, distilling out most of ethyl acetate, reducing the pressure when the material temperature reaches 150 ℃, keeping the temperature at 150 ℃ for 1.5h to obtain white powdery MQ silicon resin, stopping reducing the pressure, adding 100 g of 20000mPa s, 0.087% double-end vinyl silicone oil and 50 g of toluene, and carrying out reduced pressure polycondensation at 150 ℃ for 3h to obtain the organic silicon pressure-sensitive adhesive base adhesive which is semitransparent viscous liquid containing transparent particles.
The silicone pressure-sensitive adhesive base obtained in comparative example 1 had a viscosity of 768000mPa · s and a vinyl mass fraction of 0.0395%.
Performance detection
The silicone pressure-sensitive adhesive base obtained in examples 1 to 11 and comparative example 1 was prepared in the same formulation ratio with hydrogen-containing silicone oil (SiH: SiVi ═ 1.2:1), platinum catalyst, and inhibitor, coated on a PET film, and cured at 120 ℃ for 5min to obtain a film having a dry adhesive thickness of 20 μm, and the initial tack, holding tack, and peel strength were measured, and the results are shown in table 5.
TABLE 5 Silicone pressure sensitive adhesive Performance test results
From the properties of the silicone pressure-sensitive adhesive prepared from the silicone pressure-sensitive adhesive-based adhesives of examples 1-4, the greater the viscosity of the double-ended vinyl silicone oil, the higher the peel strength, and when the viscosity is 5000-1000mPa · s, the initial viscosity is 10-11#, the sustained viscosity is higher than 72h, and the peel strength is 5-6N/25 mm.
From the properties of the silicone pressure-sensitive adhesives prepared from the silicone pressure-sensitive adhesive-based adhesives of examples 5-8, the peel strength of the silicone pressure-sensitive adhesive is effectively improved when polycondensation occurs under weakly alkaline conditions, i.e., at a pH of 8-9. From the performance of the silicone pressure-sensitive adhesive prepared from the silicone pressure-sensitive adhesive base adhesives of examples 9-12, the polycondensation temperature also has a great influence on the performance of the final silicone pressure-sensitive adhesive, i.e. when the polycondensation temperature is 150-.
It is known from examples 1 to 12 and comparative example 1 that when conventional toluene is used as a polycondensation medium, the molecular weight of MQ silicone resin is easily increased to make it poor in compatibility with vinyl silicone oil, and the adhesive property of silicone pressure-sensitive adhesive is seriously affected.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (10)
1. The preparation method of the organic silicon pressure-sensitive adhesive base adhesive is characterized by comprising the following steps:
1) preparing MQ silicon resin prepolymer solution;
2) and (3) reduced pressure polycondensation: adding vinyl silicone oil into the MQ silicone resin prepolymer solution in the step 1), heating, and carrying out reduced pressure polycondensation at the temperature of 120 ℃ and 180 ℃ for 1-6h to obtain the organic silicon pressure-sensitive adhesive base adhesive.
2. The method for preparing silicone pressure-sensitive adhesive-based according to claim 1, wherein in step 1), the MQ silicone resin prepolymer solution is prepared by the specific steps of: mixing polysilicate, hexamethyldisiloxane, glacial acetic acid and concentrated sulfuric acid at room temperature for 0.5-2h, heating to reflux for 3-6h, cooling, adjusting pH, and layering, wherein the organic phase is MQ silicon resin prepolymer solution.
3. The method for preparing the silicone pressure-sensitive adhesive-based according to claim 1, wherein in step 1), the molar ratio of hexamethyldisiloxane, polysilicate and glacial acetic acid is 0.3-0.6: 1: 2.0 to 2.4, and the using amount of concentrated sulfuric acid is 1.0 to 3.0 percent of the total mass of hexamethyldisiloxane and polysilicate.
4. The method for preparing the silicone pressure-sensitive adhesive-based adhesive according to claim 1, wherein in step 1), the polysilicate is polyethyl silicate and SiO is used2The mass fraction is 30-50%.
5. The method for preparing the silicone pressure-sensitive adhesive-based glue according to claim 1, wherein in step 1), the pH is adjusted to 7 to 9.
6. The method for preparing silicone pressure-sensitive adhesive-based according to claim 4, wherein in step 2), the mass ratio of the MQ silicone resin prepolymer to the vinyl silicone oil is 1: 0.5-10.
7. The method for preparing the silicone pressure-sensitive adhesive-based adhesive according to claim 1, wherein the vinyl silicone oil is a terminal vinyl polydimethylsiloxane, the viscosity thereof is in the range of 2000-50000mPa s, and the vinyl mass fraction is 0.08-0.25%.
8. The method for preparing the silicone pressure-sensitive adhesive-based adhesive as claimed in claim 1, wherein in step 2), the polycondensation is carried out at 150-160 ℃ under reduced pressure for 1-3 h.
9. The method for preparing the silicone pressure-sensitive adhesive-based adhesive according to claim 1, wherein in step 2), the pressure-reducing polycondensation is carried out until the viscosity of the silicone pressure-sensitive adhesive-based adhesive is 5000-1000000 mPa-s.
10. A silicone pressure-sensitive adhesive-based adhesive obtained by the method for preparing a silicone pressure-sensitive adhesive-based adhesive according to any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010026035.8A CN111139027B (en) | 2020-01-10 | 2020-01-10 | Organic silicon pressure-sensitive adhesive-based adhesive and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010026035.8A CN111139027B (en) | 2020-01-10 | 2020-01-10 | Organic silicon pressure-sensitive adhesive-based adhesive and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111139027A true CN111139027A (en) | 2020-05-12 |
| CN111139027B CN111139027B (en) | 2022-08-05 |
Family
ID=70524587
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010026035.8A Active CN111139027B (en) | 2020-01-10 | 2020-01-10 | Organic silicon pressure-sensitive adhesive-based adhesive and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111139027B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112280528A (en) * | 2020-09-25 | 2021-01-29 | 广东标美硅氟新材料有限公司 | Organic silicon pressure-sensitive adhesive with high peel strength and preparation method thereof |
| CN112280529A (en) * | 2020-09-25 | 2021-01-29 | 广东标美硅氟新材料有限公司 | Organosilicon skin glue and preparation method thereof |
| CN112812738A (en) * | 2020-12-30 | 2021-05-18 | 广州市瑞合新材料科技有限公司 | Organic silicon pressure-sensitive adhesive and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5602214A (en) * | 1993-05-13 | 1997-02-11 | General Electric Company | Silicone pressure-sensitive adhesive compositions |
| CN104152104A (en) * | 2014-08-21 | 2014-11-19 | 岳胜武 | Self-adhesive organic silicon press-sensitive adhesive and preparation method thereof |
| CN105585714A (en) * | 2015-12-16 | 2016-05-18 | 东莞兆舜有机硅科技股份有限公司 | Anti-ultraviolet organic silicon resin, preparation method and application thereof |
| CN106398636A (en) * | 2016-08-31 | 2017-02-15 | 湖北新四海化工股份有限公司 | Environment-friendly organosilicone pressure-sensitive adhesive and preparation method thereof |
| CN106833502A (en) * | 2016-12-29 | 2017-06-13 | 深圳市安品有机硅材料有限公司 | Peelable organic pressure-sensitive gel, pressure sensitive adhesive product and preparation method thereof |
-
2020
- 2020-01-10 CN CN202010026035.8A patent/CN111139027B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5602214A (en) * | 1993-05-13 | 1997-02-11 | General Electric Company | Silicone pressure-sensitive adhesive compositions |
| CN104152104A (en) * | 2014-08-21 | 2014-11-19 | 岳胜武 | Self-adhesive organic silicon press-sensitive adhesive and preparation method thereof |
| CN105585714A (en) * | 2015-12-16 | 2016-05-18 | 东莞兆舜有机硅科技股份有限公司 | Anti-ultraviolet organic silicon resin, preparation method and application thereof |
| CN106398636A (en) * | 2016-08-31 | 2017-02-15 | 湖北新四海化工股份有限公司 | Environment-friendly organosilicone pressure-sensitive adhesive and preparation method thereof |
| CN106833502A (en) * | 2016-12-29 | 2017-06-13 | 深圳市安品有机硅材料有限公司 | Peelable organic pressure-sensitive gel, pressure sensitive adhesive product and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112280528A (en) * | 2020-09-25 | 2021-01-29 | 广东标美硅氟新材料有限公司 | Organic silicon pressure-sensitive adhesive with high peel strength and preparation method thereof |
| CN112280529A (en) * | 2020-09-25 | 2021-01-29 | 广东标美硅氟新材料有限公司 | Organosilicon skin glue and preparation method thereof |
| CN112280529B (en) * | 2020-09-25 | 2023-11-03 | 广东标美硅氟新材料有限公司 | Organosilicon skin adhesive and preparation method thereof |
| CN112812738A (en) * | 2020-12-30 | 2021-05-18 | 广州市瑞合新材料科技有限公司 | Organic silicon pressure-sensitive adhesive and preparation method thereof |
| CN112812738B (en) * | 2020-12-30 | 2021-11-09 | 广州市瑞合新材料科技有限公司 | Organic silicon pressure-sensitive adhesive and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111139027B (en) | 2022-08-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111139027B (en) | Organic silicon pressure-sensitive adhesive-based adhesive and preparation method thereof | |
| US9926410B2 (en) | Organosiloxane compositions and coatings, manufactured articles, methods and uses | |
| CN110305486B (en) | Organic silicon gel and preparation method thereof | |
| CN102174309B (en) | Solvent-free organic silicon pressure-sensitive adhesive and preparation method thereof | |
| CN101177596B (en) | Emulsion type organic silica pressure-sensitive gel and preparation method thereof | |
| US9346954B2 (en) | Curable resin composition | |
| CN101679821B (en) | Adhesives | |
| CN101573421A (en) | Laminates utilizing pressure sensitive adhesive composition and conventional silicone liners | |
| CN105001422B (en) | A kind of addition-type silicon rubber tackifier and preparation method thereof and addition-type silicon rubber | |
| CN102876249A (en) | Preparation method of peelable type organosilicon pressure-sensitive adhesive | |
| EP2733160A1 (en) | Organo polysiloxane, and method for producing same | |
| CN103409103A (en) | Environment-friendly high-temperature-resistant organic silicon pressure-sensitive adhesive and preparation method thereof | |
| US10160859B2 (en) | Thermoplastic composition comprising a polyamide and a polysiloxane | |
| CN114574097B (en) | Bi-component normal-temperature curing epoxy modified MQ silicon resin coating | |
| CN107163252A (en) | A kind of Methyl Hydrogen Polysiloxane Fluid and purposes | |
| US4943620A (en) | Method for the preparation of a silicone-based pressure-sensitive adhesive | |
| CN112280528A (en) | Organic silicon pressure-sensitive adhesive with high peel strength and preparation method thereof | |
| CN103289095A (en) | A synthesis method of high viscosity alpha, omega-dihydroxy polydimethylsiloxane | |
| JP4772858B2 (en) | Silicone resin composition | |
| CN103665381B (en) | Synthesis method of hydroxyl capped polydimethylsiloxane | |
| CN102585234B (en) | Macromolecular coupling agent, preparation method and application thereof | |
| CN112778965B (en) | Alcohol-type silicon rubber adhesive and preparation method thereof | |
| CN115505367A (en) | High-strength organic silicon adhesive and preparation method thereof | |
| CN116496754A (en) | Single-component addition type silicone rubber with excellent adhesion to inert difficult-to-adhere base material and preparation method thereof | |
| CN111621016A (en) | Organic silicon polymer and preparation method thereof, adhesive and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |