CN108192356B - Carrier type organic silicon adhesion promoter and preparation method thereof - Google Patents
Carrier type organic silicon adhesion promoter and preparation method thereof Download PDFInfo
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Abstract
The invention provides a carrier type organic silicon adhesion promoter and a preparation method thereof, wherein the carrier type organic silicon adhesion promoter is prepared from the following components in parts by weight: 10-50 parts of ethyl orthosilicate, 1-10 parts of aminopropyltrimethoxysilane, 1-10 parts of glycidyl ether methyldimethoxysilane, 1-10 parts of aminoethylaminopropyltrimethoxysilane, 1-10 parts of aminoethylaminopropylmethyldimethoxysilane, 0.1-2 parts of catalyst, 0.1-2 parts of neutralizer, 1-3 parts of dispersant, 1-50 parts of carrier, 1-5 parts of stabilizer and 1-10 parts of water. The carrier type organic silicon adhesion promoter prepared by the invention greatly improves the surface adhesion of plastic products, and the material can modify plastics in a physical blending extrusion mode, thereby improving the surface adhesion of the plastics and improving the hand feeling and the wear resistance of the products.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to a carrier type organic silicon adhesion promoter and a preparation method thereof.
Technical Field
In recent ten years, the plastic industry in China is rapidly developed, the engineering plastics widely applied in China comprise ABS, PG, PA and POM, and the general plastics comprise PS, PC, PP, PVC and the like. The plastic product has light weight, excellent physical and chemical properties and easy mass production, and becomes an indispensable material for national economy and people's life.
The plastic is amorphous polymer, has good comprehensive performance, and can carry out secondary processing on plastic products, thereby being widely applied to products such as household appliances, foods, toys, medical treatment and the like. However, since the plastics such as PP or PE are nonpolar materials and have extremely low surface energy, it is difficult to perform painting and coating treatment on the surface layer, which affects the requirements of subsequent customers on appearance and surface performance.
The coating can adhere to the PP plastic due to the presence of two effects. One is a physical and mechanical action, the surface of the PP plastic product has a uniform micro-rough structure, after the coating is sprayed on the micro-rough surface, the coating can invade into micro-rough holes in a liquid state, after the coating is dried, the coating is crosslinked, and a paint film is nailed on the PP plastic product like a nail, which is a mechanical anchoring and locking effect. The other is chemical bond action, PP molecule contains certain polar groups, and the polar groups are activated due to the erosion of solvent in the coating to form chemical bonds with some polar groups in the coating, and the two are crosslinked with the curing of the coating. Meanwhile, the corrosion of the solvent in the coating also enables the surface of the PP plastic to generate pits, thereby creating conditions for mechanical anchoring and locking effects.
Disclosure of Invention
Technical problem to be solved
In order to solve the problems, the invention aims to provide a carrier type organic silicon adhesion promoter capable of greatly improving the surface adhesion of plastic products, and the material can modify plastics in a physical blending extrusion mode, improve the surface adhesion of the plastics, and improve the hand feeling and the wear resistance of the products.
(II) technical scheme
The invention provides a carrier type organic silicon adhesion promoter, which is prepared from the following components in parts by weight: 10-50 parts of ethyl orthosilicate, 1-10 parts of aminopropyltrimethoxysilane, 1-10 parts of glycidyl ether methyldimethoxysilane, 1-10 parts of aminoethylaminopropyltrimethoxysilane, 1-10 parts of aminoethylaminopropylmethyldimethoxysilane, 0.1-2 parts of catalyst, 0.1-2 parts of neutralizer, 1-3 parts of dispersant, 1-50 parts of carrier, 1-5 parts of stabilizer and 1-10 parts of water.
Further, in the above-mentioned case,
the catalyst is citric acid and formic acid.
The neutralizer is potassium hydroxide or sodium hydroxide.
The carrier is one or more of white carbon black, calcium carbonate, polyethylene glycol, diatomite and carbon black.
The stabilizer is one or more of sodium carboxymethylcellulose, anhydrous calcium chloride and anhydrous calcium carbonate.
The dispersing agent is organic silicon modified polyether.
The second aspect of the invention provides a preparation method of a carrier type organic silicon adhesion promoter, which sequentially comprises the following steps:
1) uniformly mixing a catalyst with tetraethoxysilane, aminopropyltrimethoxysilane and aminoethylaminopropyltrimethoxysilane, slowly dropwise adding a mixture of water and glycidyl ether methyldimethoxysilane for 1 hour, after dropwise adding, adding aminoethylaminopropyldimethoxysilane, heating to 75 ℃, carrying out reflux reaction for 3 hours, wherein a reaction product is a light yellow transparent liquid, carrying out reduced pressure distillation, adding a neutralizing agent, neutralizing, and filtering to obtain an organic silicon adhesion promoter;
2) adding the carrier into a kneader, heating to 100 ℃, vacuumizing, stirring for 1 hour, cooling to 70 ℃, adding the dispersing agent, stirring for 0.5 hour, adding the organosilicon adhesion promoter in batches, stirring to form uniform powder, adding the stabilizer after no agglomeration phenomenon, and stirring uniformly to obtain the carrier type organosilicon adhesion promoter.
The third aspect of the invention provides a plastic containing the carrier-type organic silicon adhesion promoter, which comprises 0.1-5 parts by weight of the carrier-type organic silicon adhesion promoter and 95-99.9 parts by weight of plastic, wherein the plastic is PC or PP.
The fourth aspect of the invention provides a preparation method of plastic containing carrier-type organic silicon adhesion promoter, which comprises the steps of blending and granulating the carrier-type organic silicon adhesion promoter and plastic particles, wherein the blending temperature is not more than 250 ℃, and the extrusion time is not more than 1 minute.
The technical scheme provided by the invention has the following beneficial effects:
1. according to the invention, through the proportion control of special functional groups and the formation of a main chain structure by using two functional groups (amino reaction activity), wherein a plurality of fulcrums of four functional groups with strong structural rigidity are involved to play a role in mechanical structure strength, and then other reactive functional groups of a part of three functional groups are connected to improve the reaction activity, so that the adhesive force between base materials can be greatly improved, and the long-term adhesive force effect, partial hand feeling and wear resistance can be provided.
2. The carrier type organic silicon adhesion promoter provided by the invention disperses the organic silicon adhesion promoter into the powder carrier through a special kneading process, and then is modified with plastic particles in a mixing extrusion manner, so that the problem of plastic adhesion is fundamentally solved, and the characteristics of hand feeling, wear resistance and the like of plastics can be improved.
3. The carrier type organic silicon adhesion promoter disclosed by the invention is simple and effective in use method, and the product is non-toxic and harmless, long in effectiveness and wide in application range.
Detailed Description
Ethyl orthosilicate is purchased from Wucheng Hengchanghehemical Co., Ltd. Aminopropyltrimethoxysilane, aminoethylaminopropyltrimethoxysilane, aminoethylaminopropylmethyldimethoxysilane were purchased from Nanjing Qiyu chemical technology Ltd. Glycidyl ether methyldimethoxysilane was purchased from caruncle morning light chemical company, ltd. Citric acid, formic acid, potassium hydroxide, sodium hydroxide were purchased from cigarette bench double reagents ltd. White carbon black, calcium carbonate, polyethylene glycol, diatomite, carbon black, sodium carboxymethylcellulose, anhydrous calcium chloride, anhydrous calcium carbonate and organic silicon modified polyether are purchased from Jiangsu Haian petrochemical industry. Low density polyethylene, taiwan plastics industries ltd. Paint, Anyang city Ririxiu paint, LLC.
Experimental column 1
1) Synthesizing an organic silicon adhesion promoter: uniformly mixing 0.1g of citric acid, 10g of tetraethoxysilane, 1g of aminopropyltrimethoxysilane and 1g of aminoethylaminopropyltrimethoxysilane, slowly and dropwise adding a mixture of 1g of water and 1g of glycidyl ether methyldimethoxysilane for 1 hour, after dropwise adding, then adding 1g of aminoethylaminopropyldimethoxysilane, heating to 75 ℃, carrying out reflux reaction for 3 hours, wherein the reaction product is a light yellow transparent liquid, carrying out reduced pressure distillation, adding 0.1g of potassium hydroxide, neutralizing and filtering to obtain the organic silicon adhesion promoter;
2) synthesizing a carrier type organic silicon adhesion promoter: adding 1-50g of white carbon black into a kneader, heating to 100 ℃, vacuumizing, stirring for 1 hour, cooling to 70 ℃, adding 1g of organic silicon modified polyether into the kneader, stirring for 0.5 hour, adding 30g of organic silicon adhesion promoter into the kneader by 3 times, stirring to form uniform powder, adding 1g of anhydrous calcium carbonate after no agglomeration phenomenon, and stirring uniformly to obtain the carrier type organic silicon adhesion promoter.
Example 2
1) Synthesizing an organic silicon adhesion promoter: uniformly mixing 2g of formic acid, 50g of ethyl orthosilicate, 10g of aminopropyltrimethoxysilane and 10g of aminoethylaminopropyltrimethoxysilane, slowly dripping a mixture of 10g of water and 10g of glycidyl ether methyldimethoxysilane for 1 hour, adding 10g of aminoethylaminopropyldimethoxysilane after dripping is finished, heating to 75 ℃, carrying out reflux reaction for 3 hours, adding 2g of sodium hydroxide, neutralizing and filtering to obtain the organic silicon adhesion promoter, wherein the reaction product is light yellow transparent liquid, and carrying out reduced pressure distillation;
2) synthesizing a carrier type organic silicon adhesion promoter: adding 50g of white carbon black into a kneader, heating to 100 ℃, vacuumizing, stirring for 1 hour, cooling to 70 ℃, adding 3g of organic silicon modified polyether into the kneader, stirring for 0.5 hour, adding 30g of organic silicon adhesion promoter into the kneader in 5 batches, stirring to form uniform powder, adding 5g of sodium carboxymethylcellulose after no agglomeration phenomenon, and stirring uniformly to obtain the carrier type organic silicon adhesion promoter.
Example 3
1) Synthesizing an organic silicon adhesion promoter: uniformly mixing 0.2g of formic acid, 20g of ethyl orthosilicate, 4g of aminopropyltrimethoxysilane and 3g of aminoethylaminopropyltrimethoxysilane, slowly dropwise adding a mixture of 6g of water and 3.5g of glycidyl ether methyldimethoxysilane for 1 hour, after dropwise adding, then adding 6.5g of aminoethylaminopropyldimethoxysilane, heating to 75 ℃, carrying out reflux reaction for 3 hours to obtain a reaction product which is a light yellow transparent liquid, carrying out reduced pressure distillation, adding 1g of sodium hydroxide, neutralizing and filtering to obtain the organic silicon adhesion promoter;
2) synthesizing a carrier type organic silicon adhesion promoter: adding 20g of white carbon black and 10g of calcium carbonate into a kneader, heating to 100 ℃, vacuumizing, stirring for 1 hour, cooling to 70 ℃, adding 1.3g of organic silicon modified polyether into the kneader, stirring for 0.5 hour, adding 30g of organic silicon adhesion promoter into the kneader in 3 batches, stirring to form uniform powder, adding 0.5g of sodium carboxymethylcellulose and 1g of anhydrous calcium chloride after no agglomeration phenomenon, and stirring uniformly to obtain the carrier type organic silicon adhesion promoter.
Example 4
1) Synthesizing an organic silicon adhesion promoter: uniformly mixing 1.1g of citric acid, 40g of tetraethoxysilane, 8g of aminopropyltrimethoxysilane and 2.5g of aminoethylaminopropyltrimethoxysilane, slowly and dropwise adding a mixture of 7g of water and 2g of glycidyl ether methyldimethoxysilane for 1 hour, after dropwise adding, then adding 3g of aminoethylaminopropyldimethoxysilane, heating to 75 ℃, carrying out reflux reaction for 3 hours to obtain a reaction product which is a light yellow transparent liquid, carrying out reduced pressure distillation, adding 0.8g of potassium hydroxide, neutralizing, and filtering to obtain an organic silicon adhesion promoter;
2) synthesizing a carrier type organic silicon adhesion promoter: adding 3g of white carbon black, 5g of calcium carbonate, 600020 g of polyethylene glycol and 5g of carbon black into a kneader, heating to 100 ℃, vacuumizing, stirring for 1 hour, cooling to 70 ℃, adding 3g of organic silicon modified polyether into the kneader, stirring for 0.5 hour, adding 30g of organic silicon adhesion promoter into the kneader in 3 batches, stirring to form uniform powder, adding 2g of sodium carboxymethylcellulose after no agglomeration, and stirring uniformly to obtain the carrier type organic silicon adhesion promoter.
Example 5
1) Synthesizing an organic silicon adhesion promoter: uniformly mixing 1.5g of formic acid, 20g of tetraethoxysilane, 3g of aminopropyltrimethoxysilane and 4g of aminoethylaminopropyltrimethoxysilane, slowly dropwise adding a mixture of 9g of water and 1g of glycidyl ether methyldimethoxysilane for 1 hour, after dropwise adding, then adding 3g of aminoethylaminopropyldimethoxysilane, heating to 75 ℃, carrying out reflux reaction for 3 hours, adding 1g of sodium hydroxide, neutralizing and filtering to obtain an organic silicon adhesion promoter, wherein the reaction product is a light yellow transparent liquid, carrying out reduced pressure distillation, and adding 1g of sodium hydroxide for neutralization;
2) synthesizing a carrier type organic silicon adhesion promoter: adding 450050 g of polyethylene glycol into a kneader, heating to 100 ℃, vacuumizing, stirring for 1 hour, cooling to 70 ℃, adding 3g of organic silicon modified polyether, stirring for 0.5 hour, adding 30g of organic silicon adhesion promoter in batches for 3 times, stirring to form uniform powder, adding 1g of stabilizer carboxymethylcellulose sodium after no agglomeration phenomenon, and stirring uniformly to obtain the carrier type organic silicon adhesion promoter.
Test examples
1. Preparation of sheet
Test examples 1 to 5: 3g of the carrier-type silicone adhesion promoter of examples 1 to 5, the common silane and 97g of polypropylene PP) particles were respectively subjected to blending granulation for 1 hour at a temperature of not more than 250 ℃ and extruded into a sheet, and the extrusion time was not more than 1 minute.
Comparative example: 3g of common silane and 97g of polypropylene (PP) particles are blended and granulated for 1 hour at the temperature of not more than 250 ℃, extruded into sheets, and the time of extrusion is not more than 1 minute.
2. Preparation of the coating
And preparing a sample by adopting a flow coating mode. The prepared sheet material with the thickness of 98mm multiplied by 3mm is wiped clean with antistatic dustproof cloth, and finish paint is sprayed to enable the finish paint to be evenly coated on the surface of the sheet material with the thickness of 2 mm. Drying at room temperature for 1h, curing in a drying oven at 130 ℃ for 2h, and cooling to obtain the coating.
The formula of the primer is as follows: the mass ratio of 1: 1, dissolving 5g of CPP in 95g of butyl tolueneacetate, standing for more than half a day, and heating to dissolve the mixture into a solution after the CPP can be fully swelled by the solvent.
The reference formula of the finish paint is as follows: 12g of fast yellow, DFA 158025 g, BS 120140 g, DF 13310 g, a proper amount of wetting dispersant, a proper amount of flatting agent, a proper amount of defoaming agent and 10g of diluent. The fineness of all the coatings is 2O-25 mu m.
3. Testing of coating Properties
The coating properties were tested 7 days after film formation.
The adhesive force performance of the coating is as follows: testing according to GB/T9286-1998;
coating pencil hardness property: testing according to GB/T6739-2006;
ethanol resistance of the coating: placing the sample plate in absolute ethyl alcohol, soaking for 1 hour at room temperature, taking out, airing, observing the change of the coating, and judging the ethanol resistance of the coating;
boiling resistance of the coating: placing the sample plate in deionized water at 80 ℃, soaking for 1 hour, taking out, airing, and observing the change of a sample coating;
wear resistance of the coating: the sample is placed under 0000# steel wool with 500g load, the sample surface is rubbed back and forth for 40 times, 0-5 scratches are recorded as excellent, 5-10 scratches are good, scratches above 10 scratches are poor, and the wear resistance of the coating is judged according to the number of scratches.
The performance is compared as follows:
and (4) conclusion: the adhesive force of the coating coated on the common PP can only reach 2-3 grades and cannot reach the expected standard, the adhesive force of the coating coated on the PP prepared by adding the accelerant is 0-1 grade and reaches the requirements of industrial products, the leveling property of the coating is good, the phenomena of shrinkage cavity and serious undercut are avoided, and the surface drying time is about 4 min. Secondly, if the resin in the test is thermoplastic acrylic resin, the adhesion of the coating is poor, and the coating soaked by the ethanol has serious peeling and falling off, which shows that the adhesion between the prepared coating and the thermoplastic acrylic resin is poor, so that the ethanol resistance of the coating is poor; however, after the adhesion promoter is added, the appearance of the cured coating is not obviously changed, but the performance change is obvious.
Claims (9)
1. A carrier type organic silicon adhesion promoter is characterized by being prepared from the following components in parts by weight: 10-50 parts of ethyl orthosilicate, 1-10 parts of aminopropyltrimethoxysilane, 1-10 parts of glycidyl ether methyldimethoxysilane, 1-10 parts of aminoethylaminopropyltrimethoxysilane, 1-10 parts of aminoethylaminopropylmethyldimethoxysilane, 0.1-2 parts of catalyst, 0.1-2 parts of neutralizer, 1-3 parts of dispersant, 1-50 parts of carrier, 1-5 parts of stabilizer and 1-10 parts of water.
2. The supported silicone adhesion promoter of claim 1, wherein the catalyst is citric acid, formic acid.
3. The carrier-type silicone adhesion promoter of claim 1, wherein the neutralizing agent is potassium hydroxide, sodium hydroxide.
4. The carrier-type silicone adhesion promoter of claim 1, wherein the carrier is one or more of white carbon black, calcium carbonate, polyethylene glycol, diatomaceous earth, and carbon black.
5. The carrier-type silicone adhesion promoter of claim 1, wherein the stabilizer is one or more of sodium carboxymethylcellulose, anhydrous calcium chloride, and anhydrous calcium carbonate.
6. The carrier-type silicone adhesion promoter of claim 1, wherein the dispersant is a silicone-modified polyether.
7. A method for preparing a supported silicone adhesion promoter as defined in any of claims 1 to 6, comprising the steps of, in order:
1) uniformly mixing a catalyst with tetraethoxysilane, aminopropyltrimethoxysilane and aminoethylaminopropyltrimethoxysilane, slowly dropwise adding a mixture of water and glycidyl ether methyldimethoxysilane for 1 hour, after dropwise adding, adding aminoethylaminopropyldimethoxysilane, heating to 50-90 ℃, carrying out reflux reaction for 3 hours to obtain a reaction product which is a light yellow transparent liquid, carrying out reduced pressure distillation, adding a neutralizing agent, neutralizing, and filtering to obtain an organic silicon adhesion promoter;
2) adding the carrier into a kneader, heating to 100 ℃, vacuumizing, stirring for 1 hour, cooling to 70 ℃, adding the dispersing agent, stirring for 0.5 hour, adding the organosilicon adhesion promoter in batches, stirring to form uniform powder, adding the stabilizer after no agglomeration phenomenon, and stirring uniformly to obtain the carrier type organosilicon adhesion promoter.
8. A plastic comprising the carrier-type silicone adhesion promoter of any one of claims 1-6, wherein the carrier-type silicone adhesion promoter comprises 0.1-5 parts by weight of the carrier-type silicone adhesion promoter and 95-99.9 parts by weight of the plastic, wherein the plastic is PC or PP.
9. A method of preparing the carrier-type silicone adhesion promoter plastic according to claim 8, comprising the steps of: and (3) blending and granulating the carrier type organic silicon adhesion promoter and the plastic particles, wherein the blending temperature is not more than 250 ℃, and the extrusion time is not more than 1 minute.
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| CN115109480A (en) * | 2022-07-25 | 2022-09-27 | 江苏海晟涂料有限公司 | High-performance middle coating for metal surface |
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