CN115785452B - Anti-fog additive for coating release agent and preparation method thereof - Google Patents
Anti-fog additive for coating release agent and preparation method thereof Download PDFInfo
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Abstract
The application relates to a release agent auxiliary material, in particular to an anti-fog additive for release agent coating and a preparation method thereof, wherein the anti-fog additive at least comprises grafts of hydrogen-containing silicone oil and vinyl silicone oil, the vinyl silicone oil at least comprises branched vinyl silicone oil, and the total mole number of vinyl in the vinyl silicone oil is 1.0-1.2 times of the total mole number of hydrosilyl in the hydrogen-containing silicone oil; the viscosity of the anti-fog additive for coating the parting agent is in the range of 1000-20000 cps. After the release agent antifogging additive is added into the release agent, the release agent antifogging additive has no obvious influence on the performance of the release agent, and can effectively reduce the phenomenon that the release agent is scattered and atomized to generate aerogel during roller coating.
Description
Technical Field
The application relates to a release agent auxiliary material, in particular to an anti-fog additive for release agent coating and a preparation method thereof.
Background
Release agents are currently important agents in industrial production that function to protect the pressure sensitive adhesive between the two surfaces from contamination and to allow the two surfaces to be easily peeled off when the two surfaces are attached.
The following requirements are imposed on the release agent in industry: 1. cannot transfer to the surface of the pressure-sensitive adhesive, otherwise the tackiness of the pressure-sensitive adhesive is affected; secondly, the use is convenient, and the drying time is short; 3. the corrosion to the die is avoided; 4. the adhesion to the material is low; 5. safe operation and no toxicity.
In the release agent, the linear vinyl silicone oil is widely used because of the advantages of stable property, no need of solvent, safety, no toxicity and the like. In the actual processing process, the linear vinyl silicone oil is usually coated on a target material by a multi-roller coating method, and along with the improvement of the coating process, the rotating speed of a coating roller in the rolling coating process is also continuously increased. Under the drive of coating roller pivoted centrifugal force, the release agent flies with atomizing form easily, forms atomizing state in the workshop, on the one hand to the security of operation process and personnel's occupational health influence, on the other hand also causes the loss of material.
Disclosure of Invention
The application relates to a release agent auxiliary material, in particular to an anti-fog additive for release agent coating and a preparation method thereof. The anti-fog additive for coating the release agent can ensure that the release agent has stronger adhesive force to the roller and the base material in the coating process, is suitable for various silicone oil release agents, reduces the atomization phenomenon of the release agent, and further plays roles in protecting factory environment, ensuring production safety, reducing material loss and the like.
The anti-fog additive for coating the release agent concretely adopts the following technical scheme:
an anti-fog additive for coating a release agent, which at least comprises grafts of hydrogen-containing silicone oil and vinyl silicone oil, wherein the vinyl silicone oil at least comprises branched vinyl silicone oil, and the total mole number of vinyl in the vinyl silicone oil is 1.0-1.2 times of the total mole number of hydrosilyl in the hydrogen-containing silicone oil;
the viscosity of the anti-fog additive for coating the release agent is in the range of 1000-20000 cps, preferably 5000-10000 cps.
After grafting reaction is carried out on branched vinyl silicone oil and hydrogen-containing silicone oil, the silicone oil with a network structure is obtained, and has the following characteristics:
firstly, the network structure has obvious influence on the property of the release agent, and the surface of the release agent does not contain active groups, so that the adhesion performance of the release agent is similar to that of the release agent, and the release agent is not easy to transfer into the pressure-sensitive adhesive. Secondly, the network structure can play a role in a structure similar to a protective net in the process of processing the release agent, so that small liquid drops are reduced to splash under the action of centrifugal force, and further atomization of the release agent in the roll coating process is reduced.
Preferably, the branched vinyl silicone oil is terminated by trialkoxy silicon groups, and the molar content of vinyl in the branched vinyl silicone oil is 0.2-1.0%; the molar content of the silicon-hydrogen bond in the hydrogen-containing silicone oil is 0.1-0.8%.
Preferably, the hydrogen-containing silicone oil is terminated by a trialkoxy silicon group, and the number average molecular weight of the hydrogen-containing silicone oil is 1000-10000.
Preferably, the viscosity of the anti-fog additive for coating the release agent is 1000 to 10000cps.
Preferably, the vinyl silicone oil comprises branched vinyl silicone oil and double-end vinyl silicone oil, wherein the intermediate chain unit of the double-end vinyl silicone oil contains dialkoxyl silicon chain units, and the mass ratio of the double-end vinyl silicone oil in the vinyl silicone oil is 10-20%.
Preferably, the double-ended vinyl silicone oil has a number average molecular weight of 1000 to 5000.
Preferably, the vinyl silicone oil further comprises 5-15% of hydroxyl end-capped vinyl silicone oil, and the intermediate chain unit of the hydroxyl end-capped vinyl silicone oil contains dialkoxy silicon chain units.
Preferably, the hydroxyl-terminated vinyl silicone oil has a number average molecular weight of 5000-10000 and a vinyl molar content of 0.5-1.5%.
In addition, the application also relates to a preparation method of the antifogging additive for the release agent coating, which comprises the following steps: firstly, carrying out catalytic grafting reaction on hydrogen-containing silicone oil and branched vinyl silicone oil, then adding double-end vinyl silicone oil for reaction, and finally adding hydroxyl end-capped vinyl silicone oil, wherein the reaction is completed.
The method comprises the following steps:
s1, carrying out catalytic grafting on hydrogen-containing silicone oil and branched vinyl silicone oil to obtain a graft of the hydrogen-containing silicone oil and the branched vinyl silicone oil; s2, keeping the reaction temperature unchanged, adding double-end vinyl silicone oil into the reaction system, and continuing to react to obtain an intermediate product; s3, slowly adding hydroxyl-terminated vinyl silicone oil within 30-60 min, then slowly cooling to 60-70 ℃, and stopping the reaction after reacting to a specific viscosity to obtain a target product.
Preferably, in the step S1, the reaction is carried out by adopting a method of stepwise heating to 90 ℃, the number of steps is 3-6, and the interval time between every two heating is 10-30 min.
The mixing amount of the antifogging additive in the release agent in the technical scheme can be 1-10%, the antifogging additive can inhibit atomization of the release agent to different degrees, has no obvious influence on the property of the silicone oil release agent, is simple to synthesize, and is suitable for industrial production.
Noun interpretation
In the present application, silicone oil refers to a polymer having a silicon-oxygen-silicon structure, which should be liquid at normal temperature.
Wherein the hydrogen-containing silicone oil has the following general formula
Wherein m is greater than or equal to 3, and n is greater than or equal to 1.
The branched vinyl silicone oil has the following general formula
Wherein p is greater than or equal to 3 and q is greater than or equal to 1.
The double-end vinyl silicone oil has the following general formula
Wherein h is more than or equal to 3,i and more than or equal to 0.
The hydroxyl-terminated vinyl silicone oil has the following general formula
Wherein w is greater than or equal to 3, and x is greater than or equal to 1.
In the application, all raw materials and equipment are common products sold in the market unless the raw materials and the equipment are separately described. The release agent used for the experiment is a commercial GS5005 condensation release agent with the viscosity of 1200cps, and the preparation formula is as follows:
g5005 condensation release agent: 100 parts;
solvent oil No. 120: 1900 parts;
adhesion promoters: 2 parts;
anti-fog agent: 50 parts;
organotin catalyst: 2 parts.
The peel strength of the release agent was determined to be 0.270N/mm without the addition of an anti-fog agent.
In the present application, the properties of the following anti-fog additives are judged by the following method:
anti-fogging properties: under clean environment, an aerosol detector is adopted to measure, and whether aerosol is detected at a certain linear velocity is measured so as to judge the anti-fogging performance of the anti-fog agent.
Under the experiment, the anti-fogging effect brought by different anti-fogging agents and different mixing ratios of the same anti-fogging agents can be judged.
And (3) measuring the performance of the release agent: specifically referring to GB/T25256-2010 test method for 180 DEG stripping force and residual adhesion rate of optical functional film-release film, the property of the release agent is determined by adopting a PET release film stripping force tester to measure the stripping strength of the release agent, wherein the thickness of the release agent after coating is 0.019mm.
The release agent is selected to be silicone oil,
in addition, for the convenience of calculation, the molar ratio estimation method of the silicon-hydrogen bond and the vinyl is as follows:
a is the mass of branched vinyl silicone oil;
MA is the vinyl mole fraction in the branched vinyl silicone oil;
b is the mass of hydroxyl end-capped vinyl silicone oil
MB is the mole fraction of vinyl in the hydroxyl-terminated vinyl silicone oil;
c is the mass of hydrogen-containing silicone oil;
MC is the mole fraction of silicon-hydrogen bond in hydrogen-containing silicone oil.
In the above calculation method, since the average molecular weight of the three silicone oils is relatively close to that of the single chain in practice, the actual calculation result is uniformly truncated and is close to that of the above calculation result under the condition of the present application.
The following examples and comparative examples illustrate the technical aspects of the present application.
Example 1, directed to an anti-mist additive, the method of preparation comprising the steps of:
s1, carrying out catalytic reaction on hydrogen-containing silicone oil and branched vinyl silicone oil under the action of a platinum catalyst, wherein the dosage of the hydrogen-containing silicone oil is 100g, the number average molecular weight is 5000, and the hydrogen molar content is 0.5%.
The mass of the platinum catalyst is 0.1 percent of the mass of the hydrogen-containing silicone oil;
the branched vinyl silicone oil has a vinyl molar content of 0.6% and a number average molecular weight of 12000; the mass used is 75g;
in this step, the temperature was stepped up from 20 ℃ (room temperature) to 90 ℃, wherein the number of temperature steps was 5, and the interval time between each two increases was 30min.
S2, adding double-end vinyl silicone oil into the system, and reacting for 30min under heat preservation;
wherein the number average molecular weight of the double-ended vinyl silicone oil is 5000, and the mass of the double-ended vinyl silicone oil is 15g.
S3, uniformly adding hydroxyl-terminated vinyl silicone oil into the system within 30-60 min, and naturally cooling to 60 ℃. The reaction was continued and the viscosity was checked until the viscosity reached 10000cps, and the reaction was terminated by rapid cooling.
Wherein the hydroxyl end-capped vinyl silicone oil has a number average molecular weight of 10000 and a vinyl molar content of 1.0%; the dosage is 10g.
The molar ratio of vinyl groups to silicon-hydrogen bonds in example 1 was calculated to be 1:1.1.
In contrast to example 1, the comparative example is as follows:
example 2 the specific preparation procedure for the anti-mist additive is as follows:
s1, changing the dosage of the branched vinyl silicone oil into 100g on the basis of the embodiment 1;
step S2 is kept unchanged, and after step S2 is finished, the temperature is naturally reduced to room temperature, and step S3 is deleted.
Example 3 differs from example 1 in that step S3 is deleted and a corresponding mass of hydroxy-terminated vinyl silicone oil is added after the end of the reaction.
Embodiment 4 differs from embodiment 1 in that step S2 is deleted.
Example 5 differs from example 1 in that step S2 is deleted and that after the end of the reaction i has cooled to room temperature, a vinyl-terminated silicone oil of corresponding mass is added.
Comparative example 1 was a combination of hydrogen-containing silicone oil, branched vinyl silicone oil, terminal vinyl silicone oil and hydroxyl-terminated vinyl silicone oil in the same mass ratio as in example 1, and was used as an antifogging agent after direct mixing.
The viscosity and anti-fogging properties of the anti-fogging additives prepared in examples 1 to 5 were measured and are shown in Table 1.
Table 1, experimental results of examples 1 to 5
In the table above, the roller speed was the surface linear speed, and the initial speed was increased by 100m/min, each time by 10m/min, until aerosol was detected by 350m/min or an aerosol detector. The same measurement method was used in the following experiments.
As is clear from the data in table 1, the above auxiliary materials were directly mixed, and therefore, the anti-fogging effect was not obtained, and in fact, the main anti-fogging effect was obtained in the composition, and the main effect was actually a network-like cross-linked structure formed by vinyl silicone oil and hydrogen-containing silicone oil. Although the network silicone oil system formed by crosslinking branched vinyl silicone oil and extruded hydrogen-containing silicone oil can effectively improve the adhesion capability of the network silicone oil system on the surface of a roller, reduce the flying fog phenomenon caused by the excessively high rotating speed of the roller, and simultaneously, the adhesion performance of the release agent is not obviously changed.
Among the components added thereto, vinyl terminated silicone oil, although not providing higher complexity in the silicone oil composite crosslinking system participating in the network structure, can provide necessary double-ended connection, thereby connecting different silicone oil network structures together, so that the antifogging agent in example 1 has significantly improved antifogging performance compared with examples 2 and 3. In the presence of hydroxyl groups, the release agent can be better transferred from the roll surface to the paper surface, which also reduces the generation of release agent fogging.
Further, the following examples can be obtained by adjusting each parameter based on example 1.
Example 6 the effect of viscosity on the results at various experimental conditions and final antifogging agent was investigated and the results obtained are shown in table 2.
Table 2, example 6 results of investigation of experimental parameters
In step S1, the degree of crosslinking of the silicone oil obtained by the preparation can be controlled better by adopting a step-wise heating mode, and in the heating mode, if the mode (6-6) of heating to 90 ℃ at one time and keeping the reaction is adopted, the too high degree of crosslinking can be generated in step S1, and the subsequent reaction can be influenced negatively. When the crosslinking degree in the step S1 is too low (e.g., 6-3 to 6-5), a better network structure cannot be realized in the subsequent reaction, and thus the prepared antifogging agent has poor antifogging performance.
Experiments 6-8 to 6-11 show that the antifogging agent can exert better antifogging effect within the viscosity range of 1000-20000 cps, has no obvious influence on the parting agent, and can be easily crosslinked with an organic phase to further increase the peeling strength.
Although the viscosity can be increased by extending the reaction time in both step S1 and step S3, even in the case where the final viscosity is the same, if sufficient crosslinking does not occur in step S1, the optimum anti-fog effect is still provided. The reason for this may be that, in step S2, after the crosslinking reaction of the terminal vinyl silicone oil and the hydrogen-containing silicone oil, the subsequent branched vinyl-containing silicone oil (whether unreacted vinyl silicone oil or hydroxyl-terminated vinyl silicone oil) is caused to be more difficult to undergo a complex crosslinking reaction with the hydrogen-containing silicone oil by the steric hindrance effect, so that the purpose of improving the anti-fog performance cannot be perfectly achieved by the internal network structure although the viscosity reaches the standard.
Based on the above, the properties and proportions of hydrogen-containing silicone oil, branched vinyl silicone oil, double-end vinyl silicone oil and hydroxyl-end vinyl silicone oil were studied for the influence on the antifogging agent, and the following experimental groups were included in detail.
Example 7 the effect of parameters such as the amount of each component, the content of functional bonds, the molar ratio of silicon-hydrogen bonds to vinyl groups, etc. on properties was studied.
7-1: 500g of hydrogen-containing silicone oil, wherein the number average molecular weight is 10000, and the molar content of silicon-hydrogen bonds is 0.1%;
the rest components are kept unchanged, and the mol ratio of vinyl and silicon-hydrogen bonds is unchanged.
7-2: compared with example 1, the hydrogen-containing silicone oil has a silicon-hydrogen bond molar content of 0.2%, a mass of 150g, a vinyl molar content of 0.2% of branched vinyl silicone oil, a mass of 80g, a vinyl molar content of 1.5% of hydroxyl-terminated vinyl silicone oil, an amount of 10g, and an amount of double-ended vinyl silicone oil of 10g.
The rest components are kept unchanged, and the mol ratio of vinyl and silicon-hydrogen bond is 1.03:1.
7-3: compared with example 1, the hydrogen-containing silicone oil has a silicon-hydrogen bond molar content of 0.2%, a mass of 180g, a vinyl molar content of 1.0% of branched vinyl silicone oil, a mass of 40g, a vinyl molar content of 0.5% of hydroxyl-terminated vinyl silicone oil, a use amount of 2.5g, and a use amount of 7.5g of double-ended vinyl silicone oil.
The rest components are kept unchanged, and the mol ratio of vinyl and silicon-hydrogen bond is 1.15:1.
7-4: compared with example 1, the hydrogen-containing silicone oil has a silicon-hydrogen bond molar content of 0.4%, a mass of 150g, a vinyl molar content of 0.6% of branched vinyl silicone oil, a mass of 65g, a vinyl molar content of 1% of hydroxyl-terminated vinyl silicone oil, a use amount of 15g, and a use amount of double-ended vinyl silicone oil of 20g.
The rest components are kept unchanged, and the mol ratio of vinyl and silicon-hydrogen bond is 1.13:1.
7-5: compared with example 1, the hydrogen-containing silicone oil has a silicon-hydrogen bond molar content of 0.8%, a mass used is 100g, a vinyl molar content of branched vinyl silicone oil is 1.0%, a mass used is 70g, a vinyl molar content of hydroxyl-terminated vinyl silicone oil is 1%, an amount used is 10g, and an amount used of double-ended vinyl silicone oil is 20g.
The rest components are kept unchanged, and the mol ratio of vinyl and silicon-hydrogen bond is 1:1.
7-6: compared with the example 1, the silicon-hydrogen bond molar content in the hydrogen-containing silicone oil is 0.5%, the mass used is 100g, the vinyl molar content of the branched vinyl silicone oil is 0.5%, the mass used is 100g, the vinyl molar content of the hydroxyl-terminated vinyl silicone oil is 1%, the dosage is 10g, and the dosage of the double-ended vinyl silicone oil is 20g.
The rest components are kept unchanged, and the mol ratio of vinyl and silicon-hydrogen bond is 1:1.
The experimental data for each set of example 7 are shown in table 3.
Table 3, experimental results in example 7
Further, on the basis of the above parameters, the influence of the molecular weight of each component on the properties of the silicone oil prepared was studied to obtain example 8, and the specific experimental groups are shown in Table 4.
Viscosity and experimental results in example 8
The data of examples 7 and 8 show that the parameter adjustment has no obvious influence on the overall anti-fog performance in the range, and better anti-fog effect can be better realized at the highest rotating speed in the prior industry, but the excessively high or excessively low overall viscosity can have a certain influence on the peel strength of the release agent.
In addition, it is not shown in the experimental data that when the amount of the hydroxyl-terminated vinyl silicone oil is too high, a part of the residual hydroxyl groups thereof may have a significant influence on the separation performance of the release agent, resulting in a significant improvement in the peel strength and thus affecting the properties of the release agent, and therefore, the amount of the hydroxyl-terminated vinyl silicone oil is not preferably more than 15% of the total amount of the vinyl silicone oil.
The above embodiments are not intended to limit the scope of the present application, so: all equivalent changes in structure, shape and principle of the application should be covered in the scope of protection of the application.
Claims (6)
1. An anti-fog additive for coating a release agent is characterized by at least comprising grafts of hydrogen-containing silicone oil and vinyl silicone oil, wherein the total mole number of vinyl groups in the vinyl silicone oil is 1.0-1.2 times of the total mole number of silicon hydrogen groups in the hydrogen-containing silicone oil;
the viscosity of the anti-fog additive for coating the parting agent is in the range of 1000-20000 cps;
wherein the vinyl silicone oil comprises branched vinyl silicone oil and double-end vinyl silicone oil, the middle chain unit of the double-end vinyl silicone oil contains dialkoxy silicon chain units, and the mass ratio of the vinyl silicone oil to the vinyl silicone oil is 10-20%;
the vinyl silicone oil also comprises 5 to 15 percent of hydroxyl end-capped vinyl silicone oil, wherein the middle chain segment of the hydroxyl end-capped vinyl silicone oil contains dialkoxy silicon chain segments,
the preparation method of the antifogging additive for the parting agent coating comprises the following steps:
s1, carrying out catalytic grafting on hydrogen-containing silicone oil and branched vinyl silicone oil by adopting a step-type heating method to 90 ℃ to obtain a graft of the hydrogen-containing silicone oil and the branched vinyl silicone oil; wherein, the number of steps is 3-6, and the interval time between every two heating is 10-30 min;
s2, keeping the reaction temperature unchanged, adding double-end vinyl silicone oil into the reaction system, and continuing to react to obtain an intermediate product;
and S3, slowly adding hydroxyl-terminated vinyl silicone oil into the intermediate product in the step S2, then cooling to 60-70 ℃, and stopping the reaction after reacting to a specific viscosity to obtain the target antifogging agent.
2. An antifogging additive for coating a release agent according to claim 1, wherein the branched vinyl silicone oil is terminated with a trialkoxy silicon group, and the molar content of vinyl in the branched vinyl silicone oil is 0.2 to 1.0%; the molar content of the silicon-hydrogen bond in the hydrogen-containing silicone oil is 0.1-0.8%.
3. An anti-fog additive for coating a release agent according to claim 1, wherein the hydrogen-containing silicone oil is terminated with a trialkoxy silicon group, and the number average molecular weight of the hydrogen-containing silicone oil is 1000 to 10000.
4. The release agent coating anti-mist additive according to claim 1, wherein the viscosity of the release agent coating anti-mist additive is 1000 to 10000cps.
5. An anti-fog additive for coating a release agent according to claim 1, wherein the number average molecular weight of the double-ended vinyl silicone oil and the branched vinyl silicone oil is 1000 to 5000.
6. The anti-fog additive for coating a release agent according to claim 1, wherein the hydroxyl-terminated vinyl silicone oil has a number average molecular weight of 5000 to 10000 and a vinyl molar content of 0.5 to 1.5%.
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