CN115090827A - Mold release agent and preparation method thereof - Google Patents
Mold release agent and preparation method thereof Download PDFInfo
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- CN115090827A CN115090827A CN202210512370.8A CN202210512370A CN115090827A CN 115090827 A CN115090827 A CN 115090827A CN 202210512370 A CN202210512370 A CN 202210512370A CN 115090827 A CN115090827 A CN 115090827A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C3/00—Selection of compositions for coating the surfaces of moulds, cores, or patterns
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Abstract
The invention relates to the field of organosilicon materials, in particular to a release agent and a preparation method thereof, wherein the release agent comprises the following components in parts by weight: 50-80% of curing film-forming emulsion, 10-25% of demoulding emulsion, 1-5% of wetting and leveling agent and the balance of water. The release agent has high construction efficiency and lasting release effect, does not influence the secondary processing of products and is green and environment-friendly.
Description
Technical Field
The invention relates to the field of organic silicon materials, in particular to a release agent and a preparation method thereof.
Background
In recent years, the release agent is widely applied as an indispensable chemical auxiliary agent in industries such as metal parts, plastic products and the like, and the currently used release agents mainly include the following: 1. oily mold release agents, typically organic solution systems of silicone oils and waxes; 2. the water-based release agent is prepared by taking one or more of silicone oil, paraffin, polyethylene wax, higher fatty acid and the like as main raw materials of the release agent, and emulsifying the raw materials by adopting a proper surfactant; 3. the solvent type semi-permanent release agent consists of an active component (a high molecular monomer or an oligomer with chemical reactivity), a cross-linking agent, a catalyst, a stabilizer and a diluent; 4. the water-based semi-permanent release agent consists of an active component (a high molecular monomer or an oligomer with chemical reactivity), a cross-linking agent, a catalyst, a stabilizer, a surfactant and deionized water. However, the conventional water-based or solvent-based release agents have problems of carbon deposition, a large number of spraying times, and an increase in volatile organic compounds, and the simple film-forming release agent has problems of a low number of release times and a poor release effect.
In the prior art, oleate, silane, liquid paraffin and an emulsifier are used, but the release agent obtained by the method has the defect of low release frequency although the storage stability is good. In addition, the aqueous release agent obtained by the method using hydroxyl-terminated polydimethylsiloxane, aminoalkyl siloxane and surfactant can improve the release times, but the release effect is poor.
Disclosure of Invention
In order to solve the technical problems, the invention provides the release agent and the preparation method thereof, and the release agent has the advantages of lasting release, stable performance, safety and environmental protection.
In one aspect, a mold release agent is provided, comprising, in parts by weight:
50-80% of solidified film-forming emulsion,
10-25% of demoulding emulsion,
1 to 5 percent of wetting and leveling agent,
The balance being water.
Further, the solidified film-forming emulsion is a mixture of polysiloxane and a surfactant, wherein the solid content of the emulsion is 5-60%, and the mass ratio of the polysiloxane to the surfactant is 100: 2 to 15.
Further, the curing film-forming emulsion is an addition curing type film-forming emulsion or a condensation curing type film-forming emulsion;
preferably, the addition type emulsion consists of vinyl-terminated silicone oil, methyl hydrogen-containing silicone oil, a first catalyst, an inhibitor and a surfactant;
or the condensed emulsion consists of hydroxyl-terminated polysiloxane, a cross-linking agent, a second catalyst and a surfactant.
Further, the mass ratio of the vinyl-terminated silicone oil, the methyl hydrogen-containing silicone oil, the first catalyst and the inhibitor is 100: 1-10: 0.01-0.1: 0.01 to 0.2;
or the mass ratio of the hydroxyl-terminated polysiloxane to the cross-linking agent to the second catalyst is 100: 1-10: 0.5 to 5.
Further, the vinyl-terminated silicone oil has a structural formula:
wherein n is 200-1000;
and/or the methyl hydrogen-containing silicone oil has the structural formula
Wherein m is 2-10, and n is 20-80;
and/or the first catalyst is one or two of a Karster catalyst and a chloroplatinic acid catalyst;
and/or the inhibitor is an alkynol compound;
and/or the hydroxyl-terminated polysiloxane has a structural formula
Wherein n is 480-2300;
and/or the cross-linking agent has a general formula of RSiXm, wherein m is 2-4, R group is one of alkyl, aryl, alkylene, amino, epoxy, methacryloxy, sulfydryl or carbamido with the carbon atom number of 1-20, and X is a hydrolyzable group;
and/or the second catalyst is one or more of organic tin, organic titanium and organic bismuth.
Further, the solid content of the demolding emulsion is 5-50%, wherein the mass ratio of the demolding agent to the surfactant is 100: 5-35;
preferably, the release agent is a silicone wax or wax.
Further, the structural formula of the organic silicon wax is as follows:
wherein, the R, R1 and R2 groups are one or a combination of methyl or alkyl or aryl with 8-30 carbon atoms, and n and m are integers of 10-200;
and/or the wax is one or more of industrial type 5#, 7#, 10#, 15#, 26#, 32#, and 50# liquid paraffin, semi-refined paraffin, microcrystalline wax, insect wax, polyethylene wax, and oxidized polyethylene wax.
Further, the structural formula of the wetting and leveling agent is as follows:
wherein x and y are polymerization degrees, and x is an integer of 10-50; y is 10-70; x + y is 20-100; r is a polyether group of-R ' O (R ' O) mH, and R ' are alkyl groups of C2-C5; m is an integer of 10 to 30.
Further, the surfactant is one or more of nonionic surfactant, anionic surfactant and cationic surfactant;
preferably, the nonionic surfactant is selected from one or more of span series, tween series, polyethylene glycol fatty acid ester, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, isomeric alcohol polyoxyethylene ether, nonylphenol polyoxyethylene ether and paraffin emulsifier;
the cationic surfactant is selected from one or more of fatty amine salt, ethanolamine salt and polyethylene polyamine salt;
the anionic surfactant is selected from one or more of anionic polyacrylamide, fatty acid salt, sulfonate, sulfate salt and phosphate salt.
The application also provides a preparation method of the release agent, which comprises the following steps:
mixing a curing film-forming agent and a surfactant, and slowly dripping water to form the curing film-forming emulsion;
mixing a release agent and a surfactant, and slowly dripping water to form the release emulsion;
and mixing the cured film-forming emulsion, the demolding emulsion, the wetting and leveling agent and water according to the weight ratio to obtain the demolding agent.
Compared with release agents sold in the market, the product of the application can improve the associativity of the release agents and the mold, reduce the accumulation of carbon deposition on the mold, improve the release efficiency and the like, improve the production efficiency of users and reduce the cost.
Compared with the prior art, the method has the following advantages:
1. the construction efficiency is high: the external phase is water, has good dilutability and spraying characteristic, is easy to use, has excellent spreadability and film forming property, can quickly form a release layer on the surface of a mold, reduces the construction time and improves the product forming speed;
2. the demolding effect is durable: compared with the traditional emulsion type release agent, due to the formation of the silicone rubber film and the action of silicone wax or wax inside and on the surface of the film, the service cycle of the release agent is greatly prolonged, and the user cost is reduced;
3. does not affect the secondary processing of the product: because the silicone rubber film is formed, the usage amount of the silicone wax or the paraffin is small, and part of the silicone wax or the paraffin still keeps a solid state at the demoulding temperature, almost no or little release agent component is brought into the surface of the product, and the secondary processing of the product is not influenced;
4. green and environment-friendly: the release agent is a water-based system, avoids the use of a solvent, has no pollution to the environment, and is safe and environment-friendly.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims thereof.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to specific embodiments of the present invention. It should be apparent that the described embodiments are only some of the embodiments of the present invention, and not all of them. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the described embodiments of the invention, are within the scope of protection of the present invention.
An embodiment of the present invention provides a mold release agent, including: 50-80% of curing film-forming emulsion, 10-25% of demoulding emulsion, 1-5% of wetting and leveling agent and the balance of water.
When the content of the cured film-forming emulsion is less than 50%, a silicone film formed after curing is too thin and nonuniform, so that the use frequency of the release agent is reduced; when the content is higher than 80%, the content of the silicon wax playing a role in demoulding is lower in the metal demoulding process, and the demoulding use times are reduced.
When the content of the demoulding emulsion (silicon wax emulsion and the like) is lower than 10 percent, the content of the silicon wax playing a demoulding role in the metal demoulding process is lower, and the demoulding effect is influenced; above 25%, a large amount of free oily components exist on the surface of the cured silicone film, which easily causes oil spots on the surface of the metal demolding part, not only reduces the product quality, but also causes waste.
When the content of the wetting and leveling agent is less than 1%, the wetting and leveling effect cannot be generated; when the content is more than 5%, the wetting and leveling effect is not improved basically, waste is caused by excessive addition, and the surface glossiness of the metal demolding part is reduced under the condition of high-temperature metal demolding.
The mold release agent is a semi-permanent emulsion mold release agent, the solidified film-forming emulsion can be formed into a film at room temperature or high temperature, and the film is mixed with a mold release emulsion with mold release property to quickly form an even and flat liquid film on the surface of a mold under the action of a wetting and leveling agent. The three-dimensional structure formed by curing the reactive groups under the action of the catalyst wraps the release agent, so that the attachment amount of the release agent on a mold is increased, and the wrapped oily substance gradually migrates to the surface of the adhesive film along with the decrease of the wax or silicone oil component on the surface of the adhesive film due to the increase of the demolding times, and the demolding times are increased due to the formation of the oil film again. Meanwhile, the compact molecular membrane formed by crosslinking has higher temperature resistance, the contact between a mold and a product is avoided, the extremely low surface energy greatly promotes the rapid flow of molten metal, and the molding of a metal product is accelerated.
In another embodiment of the invention, the cured film-forming emulsion is a mixture of polysiloxane and a surfactant, wherein the solid content of the emulsion is 5-60%, and the mass ratio of the polysiloxane to the surfactant is 100: 2 to 15.
When the content of the surfactant is less than the above ratio, a critical micelle concentration cannot be formed, and the polysiloxane cannot be emulsified; when the content of the surfactant is larger than the above proportion, the viscosity of the emulsion formed by emulsification is greatly improved, so that subsequent mixing is difficult, the finally formed emulsion is not uniform enough, and the subsequent demoulding use is influenced;
when the solid content mass ratio is less than 5%, the moisture is high, the surface of the film is easy to crack, and the wrinkles cannot form a complete film; when the viscosity is more than 60%, the sample has high viscosity, and the film thickness is not uniform during film forming due to difficult leveling, so that the effect is influenced.
In another embodiment of the present invention, the cured film-forming emulsion is an addition-curable film-forming emulsion.
The addition curing type film-forming emulsion consists of an internal phase and a surfactant, wherein the internal phase consists of vinyl-terminated silicone oil, methyl hydrogen-containing silicone oil, a first catalyst and an inhibitor; the mass ratio of each component in the inner phase is 100: 1-10: 0.01-0.1: 0.01 to 0.2.
When the ratio of each reactant is out of this range, there are cases where curing is impossible, curing is incomplete, and crosslinking is excessive, and in each case, the quality of the film is deteriorated, and the number of times of use of the release agent is greatly reduced, thereby affecting the releasing effect.
Further, the structural formula of the vinyl-terminated silicone oil is shown in the specification
the methyl hydrogen-containing silicone oil has the structural formula
the first catalyst is a Karster catalyst or a chloroplatinic acid catalyst;
and/or the inhibitor is an alkynol compound.
In another embodiment of the present invention, the cured film-forming emulsion is a condensation curable film-forming emulsion.
The condensed emulsion consists of an inner phase and a surfactant, wherein the inner phase consists of hydroxyl-terminated polysiloxane, a cross-linking agent and a second catalyst. Wherein the mass ratio of the hydroxyl-terminated polysiloxane, the cross-linking agent and the second catalyst is 100: 1-10: 0.5 to 5.
When the proportion of the reactants is not in the range, incomplete condensation or raw material waste is caused, so that the film forming effect is poor, and the coating effect on the release agent is poor, for example, the release agent is not coated on the surface of a film due to the fact that the release agent is completely coated, so that the release effect is poor; or the release agent is wrapped less, so that the release agent on the surface is higher, oil spots appear on the surface of a released part, the glossiness of the surface of the part is reduced, and the product quality is influenced.
Further, the structural formula of the hydroxyl-terminated polysiloxane is shown in the specification
Wherein n is 480 to 2300.
In another embodiment of the invention, the cross-linking agent has a general formula of RSiXm, wherein m is 2-4, R is one of alkyl, aryl, alkylene, amino, epoxy, methacryloxy, mercapto or ureido with 1-20 carbon atoms, and X is a hydrolyzable group; wherein the hydrolyzable group may be a hydrolyzable group such as chlorine, alkoxy, acyloxy, amino, or the like; such as methyltrimethoxysilane, methyltriethoxysilane, terminal vinyltrimethoxysilane, terminal vinyltriethoxysilane, propyltriethoxysilane, butyltriethoxysilane, octyltriethoxysilane, or a mixture thereof; the second catalyst is one of organic tin, organic titanium and organic bismuth.
In another embodiment of the invention, the solid content of the demolding emulsion is 5-50%, wherein the mass ratio of the demolding agent to the surfactant is 100: 5-35;
similarly, when the solid content is less than 5%, the moisture content is high, which causes the final sample to form a film too slowly or not, and when the solid content is more than 50%, the viscosity of the demoulding emulsion system is high, which is not beneficial to subsequent demoulding.
When the proportion of the surfactant is less than the above proportion, the emulsion is impossible or the stability after the emulsion is poor; when the proportion of the surfactant is larger than the above proportion, excessive surfactant can cause a ten-percent obvious thickening effect on the system, so that the viscosity of the system is higher, the components are not uniformly mixed, the coating effect is not good, and the demolding effect is poor.
Further, the release agent is silicone wax or wax.
Wherein the structural formula of the organic silicon wax is shown in the specification
the wax is one or more of industrial liquid paraffin, semi-refined paraffin, microcrystalline wax, insect wax, polyethylene wax and oxidized polyethylene wax of 5#, 7#, 10#, 15#, 26#, 32#, and 50 #.
In another embodiment of the present invention, the structural formula of the wetting and leveling agent is:
The surfactant is one or more of nonionic surfactant, anionic surfactant and cationic surfactant;
preferably, the nonionic surfactant is selected from one or more of span series, tween series, polyethylene glycol fatty acid ester, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, isomeric alcohol polyoxyethylene ether, nonylphenol polyoxyethylene ether and paraffin wax emulsifier;
the cationic surfactant is selected from one or more of fatty amine salt, ethanolamine salt and polyethylene polyamine salt;
the anionic surfactant is selected from one or more of anionic polyacrylamide, fatty acid salt, sulfonate, sulfate ester salt and phosphate ester salt.
The invention also provides a preparation method of the release agent, which comprises the following steps:
mixing a solidified film-forming agent and a surfactant, and dripping water drop by drop to mix to form the solidified film-forming emulsion;
mixing a release agent and a surfactant, and dropwise adding water to mix to form the release emulsion;
and mixing the cured film-forming emulsion, the demolding emulsion, the wetting and leveling agent and water according to the weight ratio to obtain the demolding agent.
Each raw material is firstly prepared into emulsion, and the emulsified components exist in the form of aqueous emulsion particles, so that the system is very favorable for homogenization after mixing; when the curing film-forming agent and the release agent are emulsified together, a uniform and stable emulsion cannot be formed.
The present invention will be described in further detail with reference to specific embodiments.
Example 1
The embodiment provides a semi-permanent emulsion type release agent, which comprises the following components:
wherein, the curing film-forming emulsion is an addition curing type, and the structural formula of the vinyl silicone oil at the inner phase end of the emulsion is as follows:
wherein n is 200; the structural formula of the methyl hydrogen-containing silicone oil is as follows:
wherein n is 20 and m is 2; the first catalyst is a Karster catalyst, and the inhibitor is 1-ethynyl cyclohexanol; the mass of the vinyl-terminated silicone oil, the mass of the methyl hydrogen-containing silicone oil, the mass of the first catalyst and the mass of the inhibitor are respectively 100g, 3g, 0.02g and 0.01 g. The solid content of the curing film-forming emulsion is 5 percent, and the mass of the polysiloxane and the surfactant is 100g and 4g respectively.
In the demoulding emulsion, the demoulding agent is organosilicon silicon wax, and the structural formula is as follows:
Wherein the surfactant used in the curing film-forming emulsion is isomeric dodecyl alcohol polyoxyethylene ether 1003 and 1007 by mass ratio of 1: 2; the surfactant used in the demoulding emulsion is tween 80 and span 60 according to the mass ratio of 2: 1;
the structural formula of the wetting and leveling agent is as follows:
wherein x is 15, y is 20, R is-R' O (R "O) m The polyether group of H, R 'and R' are both ethyl; m is an integer of 15.
The preparation method of the release agent comprises the following steps:
mixing the vinyl-terminated silicone oil, methyl hydrogen-containing silicone oil, catalyst, inhibitor and surfactant in parts by weight, and slowly dripping water until phase inversion is carried out to obtain the curing film-forming emulsion.
Mixing the organic silicon wax and a surfactant, and slowly dripping water until phase inversion is carried out to obtain demoulding emulsion;
and uniformly stirring 50g of the cured film-forming emulsion, 10g of the demolding emulsion, 1g of the wetting and leveling agent and 39g of water to obtain the demolding agent.
Example 2
The embodiment provides a semi-permanent emulsion type release agent, which comprises the following components:
the curing film-forming emulsion is an addition curing type, and the structural formula of the vinyl silicone oil at the inner phase end of the emulsion is as follows:
wherein n is 350; the structural formula of the methyl hydrogen-containing silicone oil is as follows:
wherein n is 41 and m is 3; the solid content of the emulsion is 30 percent, and the mass of the polysiloxane and the surfactant is 100g and 2g respectively; the surfactant is octyl phenol polyoxyethylene ether OP10 and OP7 according to the mass ratio of 1: 1.
The release agent is organic silicon wax, and the structural formula of the release agent is as follows:
wherein R1 and R2 are both methyl, and R is
The surfactant is isomeric alcohol polyoxyethylene ether-7 and tween 80 according to the mass ratio of 1: the compound of 1, the weight of the organic silicon wax and the surfactant are 100g and 15g respectively, and the solid content is 20 percent.
The structural formula of the wetting and leveling agent is as follows:
wherein x is 10, y is 25, and R is-R' O (R "O) m The polyether group of H, R 'and R' are both ethyl; m is 20.
The first catalyst is a Kaster catalyst, and the inhibitor is 1-ethynylcyclohexanol; the mass of the vinyl terminated silicone oil, the mass of the methyl hydrogen-containing silicone oil, the mass of the first catalyst and the mass of the inhibitor are respectively 100g, 1g, 0.05g and 0.01 g.
The preparation method is the same as example 1.
Example 3
The embodiment provides a semi-permanent emulsion type release agent, which comprises the following components:
wherein the emulsion with the property of curing and film forming is an addition curing type, and the structural formula of the vinyl silicone oil at the inner phase end of the emulsion is as follows:
wherein n is 380; the structural formula of the methyl hydrogen-containing silicone oil is as follows:
wherein n is 60, m is 10; the solid content of the emulsion is 40 percent, and the mass of the polysiloxane and the surfactant is 100g and 6g respectively; the surfactant is isomeric dodecyl alcohol polyoxyethylene ether 1003 and 1007 according to the mass ratio of 1: 2.
The wax is industrial type 10# liquid paraffin, the surfactant is a span 60 and 1831 compound, the mass of the wax and the surfactant is 100g and 15g respectively, and the solid content is 5%.
The structural formula of the wetting and leveling agent is as follows:
wherein x is 15, y is 10, R is a polyether group of-R 'O (R' O) mH, R 'is ethyl and R' is propyl; m is an integer of 10.
The first catalyst is a chloroplatinic acid catalyst, and the inhibitor is 3, 5-dimethyl-1-hexyne-3-ol; the mass of the vinyl-terminated silicone oil, the methyl hydrogen-containing silicone oil, the first catalyst and the inhibitor is 100g, 10g, 0.03g and 0.01g respectively.
The preparation method is the same as the example.
Example 4
This example provides a semi-permanent emulsion release agent, which is composed of the following components:
the curing film-forming emulsion is an addition curing type, and the structural formula of the vinyl silicone oil at the inner phase end of the emulsion is as follows:
wherein n is 200; the structural formula of the methyl hydrogen-containing silicone oil is as follows:
wherein n is 20 and m is 8; the solid content of the emulsion is 40 percent, and the mass of the polysiloxane and the surfactant is 100g and 6g respectively; the surfactant is isomeric dodecyl alcohol polyoxyethylene ether 1003 and 1007 according to the mass ratio of 1: 2.
The wax is a mixture of industrial type No. 26 liquid paraffin and insect wax, the surfactant is a span 60 and 1831 compound, the mass of the wax and the surfactant is 100g and 15g respectively, and the solid content of the emulsion is 15%.
The structural formula of the wetting and leveling agent is as follows:
wherein x is 20, y is 60, R is a polyether group of-R 'O (R' O) mH, R 'and R' are both propyl; m is 15.
The first catalyst is a chloroplatinic acid catalyst, and the inhibitor is 3,7, 11-trimethyldodecyne-3-ol; the weight of the vinyl-terminated silicone oil, the methyl hydrogen-containing silicone oil, the first catalyst and the inhibitor is 100g, 8g, 0.1g and 0.2g respectively.
The preparation method is the same as that of example 1.
Example 5
The embodiment provides a semi-permanent emulsion type release agent, which comprises the following components:
wherein the emulsion with the property of curing and film forming is an addition curing type, and the structural formula of the vinyl silicone oil at the inner phase end of the emulsion is as follows:
wherein n is 1000; the structural formula of the methyl hydrogen-containing silicone oil is as follows:
wherein n is 80 and m is 2; the solid content of the emulsion is 50 percent, and the mass of the polysiloxane and the surfactant is 100g and 10g respectively; the surfactant is PEG4000 and 1007 according to the mass ratio of 1: 2.
The structural formula of the organosilicon silicone wax is as follows:
wherein R2 is
R, R1 are all
The wax is industrial type 32# liquid paraffin; the surfactant is a compound of a paraffin emulsifier and nonylphenol polyoxyethylene ether, and the mass of the wax, the mass of the organic silicon wax and the mass of the surfactant are respectively 100g and 35 g; the emulsion had a solids content of 50%.
The structural formula of the wetting and leveling agent is as follows:
wherein x is 30, y is 45, R is a polyether group of-R 'O (R' O) mH, R 'is propyl, R' is pentyl; m is an integer of 30.
The first catalyst is a Karster catalyst, and the inhibitor is 3,7, 11-trimethyldodecyn-3-ol; the mass of the vinyl-terminated silicone oil, the mass of the methyl hydrogen-containing silicone oil, the mass of the first catalyst and the mass of the inhibitor are respectively 100g, 7g, 0.01g and 0.2 g.
Example 6
The embodiment provides a semi-permanent emulsion type release agent, which comprises the following components:
wherein the emulsion with film-forming property is condensation-curable type, and the internal phase is
Wherein n is 480; the cross-linking agent is gamma-glycidol ether oxypropyl trimethoxy silane; the solid content of the emulsion is 30 percent, and the mass of the polysiloxane and the surfactant is 100g and 5g respectively; the surfactant is isomeric dodecyl alcohol polyoxyethylene ether 1003 and AEO3 according to the mass ratio of 2: 1.
The structural formula of the organosilicon silicone wax is as follows:
wherein R is
Wherein R1 is
R2 is methyl; the surfactant is AEO-3 and 1831 according to the mass ratio of 1: 3, the mass of the organic silicon wax and the surfactant are respectively 100g and 5g, and the solid content of the emulsion is 30 percent.
The structural formula of the wetting and leveling agent is as follows:
wherein x is 10, y is 70, R is a polyether group of-R 'O (R' O) mH, R 'is pentyl, R' is ethyl; m is an integer of 10.
The second catalyst is dibutyltin dilaurate, and the mass of the hydroxyl-terminated polysiloxane, the mass of the cross-linking agent and the mass of the second catalyst are 100g, 3g and 0.5g respectively.
The preparation method is the same as that of example 1.
Example 7
The embodiment provides a semi-permanent emulsion type release agent, which comprises the following components:
wherein the solidified film-forming emulsion is of condensation solidification type and has an internal phase of
Wherein n is 850; the cross-linking agent is gamma-glycidyl ether oxypropyl triethoxysilane; the solid content of the emulsion is 35 percent, and the mass of the polysiloxane and the surfactant is 100g and 7g respectively; the surfactant is isomeric dodecyl alcohol polyoxyethylene ether 1003 and 1007 according to the mass ratio of 1: 2.
Of silicone-silicone waxesThe structural formula is as follows:
wherein R is
R1 is methyl, R2 is
The surfactant is TO-5 and ricinoleic acid ester according TO the mass ratio of 1: 1, the mass of the organic silicon wax and the surfactant are 100g and 10g respectively, and the solid content of the emulsion is 40 percent.
The structural formula of the wetting and leveling agent is as follows:
wherein x is 20, y is 20, R is a polyether group of-R 'O (R' O) mH, R 'is ethyl, R' is propyl; m is an integer of 17.
The second catalyst is dibutyltin dilaurate, and the mass of the hydroxyl-terminated polysiloxane, the mass of the cross-linking agent and the mass of the second catalyst are respectively 100g, 1g and 0.6 g.
The preparation method is the same as that of example 1.
Example 8
The embodiment provides a semi-permanent emulsion type release agent, which comprises the following components:
wherein the solidified film-forming emulsion is of condensation solidification type and has an internal phase of
Wherein n is 1200; the cross-linking agent is N- (beta-aminoethyl) -gamma-aminopropyltrimethylsilane; the solid content of the emulsion is 40 percent, and the mass of the polysiloxane and the surfactant is 100g and 10g respectively; surface active agentOctyl phenol polyoxyethylene ether OP10 and OP7 are mixed according to the mass ratio of 1: 1. .
The wax is a mixture of industrial type No. 32 liquid paraffin and polyethylene wax, the surfactant is a compound of fatty alcohol polyoxyethylene ether (AEO-5) and sodium dodecyl benzene sulfonate, the solid content of the emulsion is 50%, and the mass of the wax and the mass of the surfactant are 100g and 20g respectively.
The structural formula of the wetting and leveling agent is as follows:
wherein x is 25, y is 20, R is a polyether group of-R 'O (R' O) mH, R 'is ethyl, R' is propyl; m is an integer of 25.
The second catalyst is bismuth neodecanoate, and the mass of the hydroxyl-terminated polysiloxane, the mass of the cross-linking agent and the mass of the second catalyst are respectively 100g, 10g and 3 g.
The preparation method is the same as that of example 1.
Example 9
The embodiment provides a semi-permanent emulsion type release agent, which comprises the following components:
wherein the solidified film-forming emulsion is of condensation solidification type and has an internal phase of
Wherein n is 1870; the cross-linking agent is octyl trimethoxy silane; the solid content of the emulsion is 60 percent, and the mass of the polysiloxane and the surfactant is 100g and 15g respectively; the surfactant is octyl phenol polyoxyethylene ether OP10 and OP7 according to the mass ratio of 1: 1. .
The wax is industrial type 15# liquid paraffin; the structural formula of the organosilicon silicone wax is as follows:
The structural formula of the wetting and leveling agent is as follows:
wherein x is 40, y is 50, R is a polyether group of-R 'O (R' O) mH, R 'and R' are both butyl; m is an integer of 15.
The second catalyst is titanate chelate, and the mass of the hydroxyl-terminated polysiloxane, the mass of the cross-linking agent and the mass of the second catalyst are respectively 100g, 8g and 5 g.
The preparation method is the same as in example 1.
Example 10
The embodiment provides a semi-permanent emulsion type release agent, which comprises the following components:
the solidified film-forming emulsion is of a condensation solidification type, and the internal phase is
Wherein n is 2300; the cross-linking agent is octyl triethoxysilane; the solid content of the emulsion is 50 percent, and the mass of the polysiloxane and the surfactant is 100g and 10g respectivelyg; the surfactant is polyoxyethylene oleate A103 and A105 according to the mass ratio of 1: 1.
The structural formula of the organosilicon silicone wax is as follows:
wherein R is methyl, R1 and R2 are both
The surfactant is a compound of castor oil phosphate and 1305, the solid content of the emulsion is 50%, and the mass of the organic silicon and the surfactant are 100g and 35g respectively.
The structural formula of the wetting and leveling agent is as follows:
wherein x is 50, y is 50, R is a polyether group of-R 'O (R' O) mH, R 'and R' are both ethyl; m is an integer of 15.
The second catalyst is dibutyltin dilaurate, and the mass of the hydroxyl-terminated polysiloxane, the mass of the cross-linking agent and the mass of the second catalyst are 100g, 10g and 3g respectively.
The preparation method is the same as that of example 1.
Comparative example 1
The same procedure as in example 1 was repeated except that no release emulsion was added.
Comparative example 2
The only release emulsion was the same as in example 1.
Comparative example 3
The procedure of example 1 was repeated except that the curing film-forming emulsion was not added.
Comparative example 4
Directly mixing the internal phase of the solidified film with a release agent, adding a surfactant and slowly dripping water until turning to form a solidified film-forming-release emulsion;
the curing film-forming-demolding emulsion, the wetting and leveling agent and water are uniformly mixed to obtain the demolding agent, and the rest is completely the same as the example 1.
Comparative example 5
The rest is the same as in example 1.
And (3) performance testing:
the emulsion stability (GB/T1603-2001) and the curing time (HG/T3947-2007) of the release agents in the above examples and comparative examples were tested to obtain Table 1:
TABLE 1 results of performance testing of examples and comparative examples (I)
All the above examples and comparative examples were subjected to demolding tests, and the number of demolds and the quality of demolded products were tested on an aluminum alloy cell phone case 1:80 (ADC12, 250T force die casting machine, mold temperature 260 ℃) to obtain Table 2.
TABLE 2 results of performance test of examples and comparative examples (II)
As can be seen from tables 1 and 2, the release agent described herein has good emulsion stability, short release time, and excellent release times.
Although the embodiments of the present invention have been described above, the above description is only for the purpose of understanding the present invention, and is not intended to limit the present invention. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The release agent is characterized by comprising the following components in parts by weight:
50-80% of solidified film-forming emulsion,
10-25% of demoulding emulsion,
1-5% of wetting and leveling agent,
The balance being water.
2. The release agent as claimed in claim 1, wherein the cured film-forming emulsion is a mixture of polysiloxane and surfactant, wherein the solid content of the emulsion is 5-60%, and the mass ratio of polysiloxane to surfactant is 100: 2 to 15.
3. The release agent claimed in claim 2 wherein the cured film-forming emulsion is an addition-curable film-forming emulsion or a condensation-curable film-forming emulsion;
preferably, the addition type emulsion consists of vinyl-terminated silicone oil, methyl hydrogen-containing silicone oil, a first catalyst, an inhibitor and a surfactant;
or the condensed emulsion consists of hydroxyl-terminated polysiloxane, a cross-linking agent, a second catalyst and a surfactant.
4. The release agent according to claim 3, wherein the mass ratio of the vinyl-terminated silicone oil, the methyl hydrogen-containing silicone oil, the first catalyst and the inhibitor is 100: 1-10: 0.01-0.1: 0.01 to 0.2;
or the mass ratio of the hydroxyl-terminated polysiloxane to the cross-linking agent to the second catalyst is 100: 1-10: 0.5 to 5.
5. The release agent as claimed in claim 4, wherein the vinyl-terminated silicone oil has a structural formula:
and/or the methyl hydrogen-containing silicone oil has the structural formula
and/or the first catalyst is one or two of a Karster catalyst and a chloroplatinic acid catalyst;
and/or the inhibitor is an alkynol compound;
and/or the hydroxyl-terminated polysiloxane has a structural formula
Wherein n is 480-2300;
and/or the cross-linking agent has a general formula of RSiXm, wherein m is 2-4, R group is one of alkyl, aryl, alkylene, amino, epoxy, methacryloxy, sulfydryl or carbamido with the carbon atom number of 1-20, and X is a hydrolyzable group;
and/or the second catalyst is one or more of organic tin, organic titanium and organic bismuth.
6. The release agent as claimed in claim 1, wherein the solid content of the release emulsion is 5 to 50%, wherein the mass ratio of the release agent to the surfactant is 100:5 to 35;
preferably, the release agent is a silicone wax or wax.
7. The release agent claimed in claim 6 wherein said silicone wax has the formula:
and/or the wax is one or more of industrial type 5#, 7#, 10#, 15#, 26#, 32#, and 50# liquid paraffin, semi-refined paraffin, microcrystalline wax, insect wax, polyethylene wax, and oxidized polyethylene wax.
8. The release agent as claimed in claim 1, wherein the wetting and leveling agent has a structural formula:
9. The release agent according to claim 2 or 6, characterized in that the surfactant is one or more of a nonionic surfactant, an anionic surfactant, a cationic surfactant;
preferably, the nonionic surfactant is selected from one or more of span series, tween series, polyethylene glycol fatty acid ester, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, isomeric alcohol polyoxyethylene ether, nonylphenol polyoxyethylene ether and paraffin emulsifier;
the cationic surfactant is selected from one or more of fatty amine salt, ethanolamine salt and polyethylene polyamine salt;
the anionic surfactant is selected from one or more of anionic polyacrylamide, fatty acid salt, sulfonate, sulfate ester salt and phosphate ester salt.
10. A method for preparing the release agent according to any one of claims 1 to 9, comprising:
mixing a curing film-forming agent and a surfactant, and slowly dripping water to form the curing film-forming emulsion;
mixing a release agent and a surfactant, and slowly dripping water to form the release emulsion;
and mixing the solidified film-forming emulsion, the demolding emulsion, the wetting and leveling agent and water according to the weight ratio to obtain the demolding agent.
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| CN116082876A (en) * | 2023-01-10 | 2023-05-09 | 杭州崇耀科技发展有限公司 | Wax-feel parting agent |
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