CN102827495A - Preparation method of high transparent precipitated silica for plastic anti-block agent - Google Patents
Preparation method of high transparent precipitated silica for plastic anti-block agent Download PDFInfo
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- CN102827495A CN102827495A CN2012103430712A CN201210343071A CN102827495A CN 102827495 A CN102827495 A CN 102827495A CN 2012103430712 A CN2012103430712 A CN 2012103430712A CN 201210343071 A CN201210343071 A CN 201210343071A CN 102827495 A CN102827495 A CN 102827495A
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Abstract
The invention discloses a preparation method of high transparent precipitated silica for plastic anti-block agent. The preparation method takes industrial sodium silicate as raw material to produce the precipitated silica which is excellent in composite indicators such as chemical purity, pore property, average particle size, volatile matter and the like so as to be used as the plastic anti-block agent. In the whole technical process, strict technical raw materials are not needed to be used, and the reaction time is 2-5h. A great deal of hydroxyl exists on the surface of the silica, and the grafting reaction is carried out between the silica and surface active material in the pulping process, so that the compatibility between the silica and polyvinyl is improved, and the transparency of the silica in the polyvinyl is remarkably improved.
Description
Technical field
The invention belongs to chemical field, be specifically related to the preparation method of a kind of plastics opening agent with high transparent precipitated silica.
Background technology
Along with high speed development of national economy; Demand rapid growth to synthetic materialss such as plastics; Drive poly production and get into a historical peak period, polyvinylidene film is widely used in aspects such as food product pack, medical packaging, cultural goods packing and agricultural film.Yet plastics film licks in journey and the storage process coiling into, owing to receive hot pressing or pressurized to be prone to stick together, makes the processing of road, back gently unreel development rate and is affected between thin film layer, and is heavy then can't launch use.The adhesion major cause of plastics film: be owing to there is a large amount of molecular chains that exposes on its surface behind the film forming, the mutual winding adhesion producing after two film closures between the macromolecular chain can't be opened it.The mutual adhesion of plastics film is used to automatic packaging and is brought difficulty; Usually in Vilaterm, add silicon-dioxide as the opening agent in order to address this problem; It makes the plastics film surface form the uneven of microcosmic, has stoped the winding between the low molecular weight substance to play anti-stick effect.Yet because silicon-dioxide itself is a kind of hydrophilic material, dispersed in Vilaterm, consistency is very poor, influence the transparency of polyvinylidene film, and then influenced poly quality.Patent CN101280127 introduces a kind of preparation method of silicon dioxide for plastic film anti-block agent.Its step is following: add water at reaction kettle, add deposition white carbon black, be warming up to 87 ℃, add the minor amount of silicon acid sodium aqueous solution earlier, transferring reacting liquid pH value is 10.2; All the other sodium silicate aqueous solutions and 20% dilute sulphuric acid add in the reaction kettle simultaneously, and the dilute sulphuric acid flow will keep pH value 10.2 constant, and 87 ℃ of temperature maintenances are constant, 85 minutes reaction times; Continue to add 22 minutes 20% dilute sulphuric acid reaction times then, adjust pH 3.8, ageing 25 minutes; Washing then, pulp, spraying drying get finished product.This method has only been investigated the opening performance of silicon-dioxide, but not to the influence to polyethylene transparency of the pore property that relates to product and granularity.And the pore property of product and mean particle size are the key factors that influences the polyvinylidene film transparency.US2765242 has introduced a kind of preparation method of precipitated silica; Whole process comprises with in the acid and water glass, and colloidal particle is grown up in weakly alkaline solution, comes the flocculated colloid particle with soluble sodium salt; Make it to assemble, need to strengthen aggregate structure simultaneously for deposition.For specific surface less than 200m
2The precipitated silica of/g can directly filter from water, and filtration cakes torrefaction promptly gets product, and for specific surface greater than 200m
2The precipitated silica of/g, the most handy alcohol or ketone displace the moisture in the aggregate, and when drying, unlikely the becoming of structure is difficult for disperseing.This patent has only been introduced the preparation method of the precipitator method, and the mean particle size to product does not describe.
Because there is a large amount of hydroxyls on the precipitated silica surface, it is very poor to be that a kind of hydrophilic material causes with poly consistency, is difficult to disperse, and therefore makes the surface property variation of plastics film.Yet along with the requirement to the sealed polyethylene plastic quality progressively improves; Performance requriementss such as its transparency, opening property and flake, tensile strength, tear strength are more and more stricter; These performances of plastics film all have direct relation with the performance of silicon-dioxide opening agent; Wherein the purity of silicon-dioxide and mean particle size are the principal elements that influences polyvinylidene film transparency and opening performance, and the pore property of silicon-dioxide has influenced the aperture efficiency of polyvinylidene film.Therefore in order to guarantee the above-mentioned performance of polyvinylidene film, the agent of silicon-dioxide opening must be satisfied the requirement of following several respects, 1) chemical purity, 2) pore property, 3) size-grade distribution.4) fugitive constituent.Must condition could use satisfying above-mentioned four as polyvinylidene film silicon-dioxide.Therefore, we have invented and have been suitable for the agent of plastics opening with high transparent precipitated silica preparation method.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of plastics opening agent with high transparent precipitated silica; The employing industrial metasilicate is a raw material; Produce precipitated silica; Its chemical purity, pore property, mean particle size, overall targets such as fugitive constituent are excellent, thereby can use as the agent of plastics opening.Whole technological process need not to use the strict process raw material, and the reaction times is 2-5 hour.Because there is a large amount of hydroxyls in silica sphere, in pulping process, carries out graft reaction with surfactant, has increased silicon-dioxide and poly consistency, and silicon-dioxide is significantly improved in poly transparency.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
The agent of a kind of plastics opening may further comprise the steps with the preparation method of high transparent precipitated silica:
(1) be the industrial metasilicate of 3.0-3.3 with modulus, the mass percent that is mixed with silicon-dioxide is the industrial metasilicate solution of 5-8%; Dripping mass percent down at 40-60 ℃ is the inorganic acid solution of 90-95%, is warming up to 80-90 ℃, is incubated 1-2 hour, and dripping the sulphur acid for adjusting pH value is 3-4;
(2) filter, washing, wash to the mass percent of sodium ion be below 0.1%;
(3) filter cake after will washing is pulled an oar with high-speed stirring, and normal temperature adds tensio-active agent down, keeps 1-1.5 hour;
(4) spraying drying, temperature out 105-110 ℃, makes product moisture keep below 3% by inlet temperature 400-600 ℃;
(5) adopt micronizer mill that dried material is pulverized and size classification, controlling its mean particle size is 3-4 μ m, obtains the finished product.
The described mineral acid of step (1) is selected from one or more of sulfuric acid, nitric acid, phosphoric acid.
The described mode of washing of step (2) is selected from one or more that washing, alcohol wash.
The described tensio-active agent of step (3) is selected from one or more of γ-r-chloropropyl trimethoxyl silane, AEO, polyoxyethylene sorbitan fatty ester, and add-on is the 1-3% of stock quality.
The index of the finished product is: silicon-dioxide>=99.4%, specific surface area: 200-300m
2/ g, mean particle size: 3-4 μ m, fugitive constituent :≤3%.
Beneficial effect of the present invention:
(1) the present invention reaches the purpose of regulating the silicon-dioxide pore property through the reaction density of regulating initial temperature, silicon-dioxide.
(2) the present invention produces precipitated silica, its chemical purity, pore property, mean particle size, and overall targets such as fugitive constituent are excellent, thereby can use as the agent of plastics opening.
(3) whole technological process of the present invention need not to use the strict process raw material, and the reaction times is 2-5 hour.Because there is a large amount of hydroxyls in silica sphere, in pulping process, carries out graft reaction with surfactant, has increased silicon-dioxide and poly consistency, and silicon-dioxide is significantly improved in poly transparency.
Embodiment
Embodiment 1
1) with modulus be 3.0 industrial metasilicate, the mass content that is diluted to concentration and is silicon-dioxide is 5% industrial metasilicate solution; Dripping mass content down 45 ℃ of initial temperatures is 95% inorganic acid solution, and mineral acid is selected from one or more of sulfuric acid, nitric acid, phosphoric acid; Add-on is 20% of a used sulfuric acid total amount, is warming up to 80-90 ℃ then, is incubated 1-1.5 hour, under this temperature, drips remaining sulfuric acid, and keeping the final pH value of regulating is 3-4;
2) wash, mode of washing is selected from washing, one or more that alcohol is washed, wash to the sodium ion mass content be below 0.1%;
3) filter cake after will washing is pulled an oar with high-speed stirring, adds tensio-active agent, and tensio-active agent is selected from γ-r-chloropropyl trimethoxyl silane, and add-on is 1%; Kept 1-1.5 hour.
4) drying, drying mode adopts spraying drying: inlet temperature keeps 400-600 ℃, and temperature out keeps 105-110 ℃, makes product moisture keep below 3%;
5) adopt micronizer mill that above-mentioned dried material is pulverized and size classification, make mean particle size: 3-4 μ m obtains the finished product.Its experimental data such as table 1.
The physical and chemical performance of table 1 silicon-dioxide opening agent embodiment
Embodiment 2
1) with modulus be 3.1 industrial metasilicate, the mass content that is diluted to concentration and is silicon-dioxide is 6% industrial metasilicate solution; Dripping mass content down 50 ℃ of initial temperatures is 95% inorganic acid solution, and mineral acid is selected from one or more of sulfuric acid, nitric acid, phosphoric acid; Add-on is 22% of a used sulfuric acid total amount, is warming up to 80-90 ℃ then, is incubated 1-1.5 hour, under this temperature, drips remaining sulfuric acid, and keeping the final pH value of regulating is 3-4;
2) wash, mode of washing is selected from washing, one or more that alcohol is washed, wash to the sodium ion mass content be below 0.1%;
3) filter cake after will washing is pulled an oar with high-speed stirring, adds tensio-active agent, and tensio-active agent is selected from AEO, and add-on is 1.5%; Kept 1-1.5 hour.
4) drying, drying mode adopts spraying drying: inlet temperature keeps 400-600 ℃, and temperature out keeps 105-110 ℃, makes product moisture keep below 3%;
5) adopt micronizer mill that above-mentioned dried material is pulverized and size classification, make mean particle size: 3-4 μ m obtains the finished product.Its experimental data such as table 2.
The physical and chemical performance of table 2 silicon-dioxide opening agent embodiment
Embodiment 3
1) with modulus be 3.2 industrial metasilicate, the mass content that is diluted to concentration and is silicon-dioxide is 7% industrial metasilicate solution; Dripping mass content down 55 ℃ of initial temperatures is 95% inorganic acid solution, and mineral acid is selected from one or more of sulfuric acid, nitric acid, phosphoric acid; Add-on is 24% of a used sulfuric acid total amount, is warming up to 80-90 ℃ then, is incubated 1-1.5 hour, under this temperature, drips remaining sulfuric acid, and keeping the final pH value of regulating is 3-4;
2) wash, mode of washing is selected from washing, one or more that alcohol is washed, wash to the sodium ion mass content be below 0.1%;
3) filter cake after will washing is pulled an oar with high-speed stirring, add tensio-active agent, and tensio-active agent is selected from AEO, polyoxyethylene sorbitan fatty ester, and add-on respectively is 0.5%; Kept 1-1.5 hour.
4) drying, drying mode adopts spraying drying: inlet temperature keeps 400-600 ℃, and temperature out keeps 105-110 ℃, makes product moisture keep below 3%;
5) adopt micronizer mill that above-mentioned dried material is pulverized and size classification, make mean particle size: 3-4 μ m obtains the finished product.Its experimental data such as table 3.
The physical and chemical performance of table 3 silicon-dioxide opening agent embodiment
Embodiment 4
1) with modulus be 3.3 industrial metasilicate, the mass content that is diluted to concentration and is silicon-dioxide is 7% industrial metasilicate solution; Dripping mass content down 60 ℃ of initial temperatures is 95% inorganic acid solution, and mineral acid is selected from one or more of sulfuric acid, nitric acid, phosphoric acid; Add-on is 25% of a used sulfuric acid total amount, is warming up to 80-90 ℃ then, is incubated 1-1.5 hour, under this temperature, drips remaining sulfuric acid, and keeping the final pH value of regulating is 3-4;
2) wash, mode of washing is selected from washing, one or more that alcohol is washed, wash to the sodium ion mass content be below 0.1%;
3) filter cake after will washing is pulled an oar with high-speed stirring, add tensio-active agent, and tensio-active agent is selected from AEO, polyoxyethylene sorbitan fatty ester, and add-on respectively is 0.5%; Kept 1-1.5 hour;
4) drying, drying mode adopts spraying drying: inlet temperature keeps 400-600 ℃, and temperature out keeps 105-110 ℃, makes product moisture keep below 3%;
5) adopt micronizer mill that above-mentioned dried material is pulverized and size classification, make ... Mean particle size: 3-4 μ m obtains the finished product.Its experimental data such as table 4.
The physical and chemical performance of table 4 silicon-dioxide opening agent embodiment
The above is merely preferred embodiment of the present invention, and all equalizations of doing according to claim of the present invention change and modify, and all should belong to covering scope of the present invention.
Claims (4)
1. plastics opening agent is characterized in that with the preparation method of high transparent precipitated silica: described preparation method may further comprise the steps:
(1) be the industrial metasilicate of 3.0-3.3 with modulus, the mass percent that is mixed with silicon-dioxide is the industrial metasilicate solution of 5-8%; Dripping mass percent down at 40-60 ℃ is the inorganic acid solution of 90-95%, is warming up to 80-90 ℃, is incubated 1-2 hour, and dripping the sulphur acid for adjusting pH value is 3-4;
(2) filter, washing, wash to the mass percent of sodium ion be below 0.1%;
(3) filter cake after will washing is pulled an oar with high-speed stirring, and normal temperature adds tensio-active agent down, keeps 1-1.5 hour;
(4) spraying drying, temperature out 105-110 ℃, makes product moisture keep below 3% by inlet temperature 400-600 ℃;
(5) adopt micronizer mill that dried material is pulverized and size classification, controlling its mean particle size is 3-4 μ m, obtains the finished product.
2. plastics opening according to claim 1 agent is characterized in that with the preparation method of high transparent precipitated silica: the described mineral acid of step (1) is selected from one or more of sulfuric acid, nitric acid, phosphoric acid.
3. plastics opening according to claim 1 agent is characterized in that with the preparation method of high transparent precipitated silica: the described mode of washing of step (2) is selected from one or more that washing, alcohol wash.
4. plastics opening according to claim 1 agent is with the preparation method of high transparent precipitated silica; It is characterized in that: the described tensio-active agent of step (3) is selected from one or more of γ-r-chloropropyl trimethoxyl silane, AEO, polyoxyethylene sorbitan fatty ester, and add-on is the 1-3% of stock quality.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103303929A (en) * | 2013-07-06 | 2013-09-18 | 福建省三明同晟化工有限公司 | Preparation method of high-transparency high-dispersity white carbon black |
| CN103911022A (en) * | 2014-04-10 | 2014-07-09 | 福建省顺昌县新和纳米硅业有限公司 | Particle size controllable nano silica and preparation method thereof |
| CN106634055A (en) * | 2016-11-29 | 2017-05-10 | 华东理工大学 | Method for emulsifying and modifying silicon dioxide at high speed |
| CN107603281A (en) * | 2017-09-14 | 2018-01-19 | 枣庄矿业（集团）有限责任公司蒋庄煤矿 | A kind of fast preparation method with white carbon black modified by silane coupling agent |
| CN111454591A (en) * | 2019-01-22 | 2020-07-28 | 北京化工大学 | Method for modifying silicon dioxide, modified silicon dioxide and application |
| CN112384475A (en) * | 2020-02-17 | 2021-02-19 | 浙江三时纪新材科技有限公司 | Preparation method of non-porous spherical silicon dioxide opening agent, thin film opening agent obtained by preparation method and application of thin film opening agent |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102532950A (en) * | 2010-12-17 | 2012-07-04 | 北京航天赛德科技发展有限公司 | Preparation method for microparticle type silica gel thin film opening agent |
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- 2012-09-17 CN CN2012103430712A patent/CN102827495A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102532950A (en) * | 2010-12-17 | 2012-07-04 | 北京航天赛德科技发展有限公司 | Preparation method for microparticle type silica gel thin film opening agent |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103303929A (en) * | 2013-07-06 | 2013-09-18 | 福建省三明同晟化工有限公司 | Preparation method of high-transparency high-dispersity white carbon black |
| CN103911022A (en) * | 2014-04-10 | 2014-07-09 | 福建省顺昌县新和纳米硅业有限公司 | Particle size controllable nano silica and preparation method thereof |
| CN103911022B (en) * | 2014-04-10 | 2016-01-20 | 福建省馨和纳米硅业有限公司 | Nano silicon of a kind of size tunable and preparation method thereof |
| CN106634055A (en) * | 2016-11-29 | 2017-05-10 | 华东理工大学 | Method for emulsifying and modifying silicon dioxide at high speed |
| CN107603281A (en) * | 2017-09-14 | 2018-01-19 | 枣庄矿业（集团）有限责任公司蒋庄煤矿 | A kind of fast preparation method with white carbon black modified by silane coupling agent |
| CN107603281B (en) * | 2017-09-14 | 2020-04-17 | 枣庄矿业（集团）有限责任公司蒋庄煤矿 | Rapid preparation method of silane coupling agent modified white carbon black |
| CN111454591A (en) * | 2019-01-22 | 2020-07-28 | 北京化工大学 | Method for modifying silicon dioxide, modified silicon dioxide and application |
| CN112384475A (en) * | 2020-02-17 | 2021-02-19 | 浙江三时纪新材科技有限公司 | Preparation method of non-porous spherical silicon dioxide opening agent, thin film opening agent obtained by preparation method and application of thin film opening agent |
| WO2021163848A1 (en) * | 2020-02-17 | 2021-08-26 | 浙江三时纪新材科技有限公司 | Preparation method for non-porous spherical silicon dioxide anti-blocking agent, thin film anti-blocking agent obtained by same, and application thereof |
| CN112384475B (en) * | 2020-02-17 | 2022-03-04 | 浙江三时纪新材科技有限公司 | Preparation method of non-porous spherical silicon dioxide opening agent, thin film opening agent obtained by preparation method and application of thin film opening agent |
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Application publication date: 20121219 |