CN102532950B - Preparation method for microparticle type silica gel thin film opening agent - Google Patents
Preparation method for microparticle type silica gel thin film opening agent Download PDFInfo
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- CN102532950B CN102532950B CN201010611813.6A CN201010611813A CN102532950B CN 102532950 B CN102532950 B CN 102532950B CN 201010611813 A CN201010611813 A CN 201010611813A CN 102532950 B CN102532950 B CN 102532950B
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Abstract
The invention relates to a preparation method for a microparticle type silica gel thin film opening agent. The preparation method mainly comprises the following steps of: adding a certain quantity of a sodium silicate aqueous solution into a reaction kettle; adding an inorganic acid solution at the initial reaction temperature and reacting; adjusting the pH value to be A; after being gelled, continuously adding the inorganic acid solution and adjusting the pH value to be B; and performing aftertreatment procedures of ageing, filtering, washing, drying and crushing to obtain the final product, namely washing by using deionized water until the pH value to be 6 to 7 after filtering, adding volatile weak acid and adjusting the pH value of the pulp to be 4 to 5, adding a 0.5 percent surface tension control agent, stirring for 5 to 10 minutes and then performing spray drying, wherein the surface tension control agent is a non-ionic silane dispersant or an organic silane coupling agent. According the method, the used materials are low in cost; the process is simple; the affinity degree of silicon dioxide particles and an organic polymer is increased; heating loss and static electricity are reduced; and the obtained product is high in purity, small in particle size and stable in performance.
Description
Technical field
The present invention relates to a kind of preparation method of silicon-dioxide, specifically relate to a kind of preparation method of the particle type silica gel for plastic film open.
Background technology
Opening agent, is that poly-bag industry is the most frequently used, indispensable auxiliary agent.Nearly all poly-bag, all contains opening agent.Opening agent is added in plastic raw materials, in film and sheet surface, form the point of a large amount of projections, form " bridge formation " phenomenon between two-layer, avoided two inner-wall surfaces to be close together on the one hand and formed " bonding " problem; Also make on the other hand air can be along opening agent the gap between the formed protruding point of film/sheet surface infiltrate through the inwall of double-layer films, to offset barometric point, thereby can effectively prevent bonding between film and the caking between pellet, improve that it is antistatic, lubricity and moisture-proof characteristic, reduce frictional coefficient and bonding resistance, and can increase the smooth finish of film surface, and prevent attached long-pending at product surface of dust, produce very smooth plastic product.
The particulate that can be used as opening agent has a variety of, and quality differs, and price differs and can reach tens times.The opening agent of par is as natural talcum powder, native silicon dioxide etc.But owing to being natural mineral matter, transparence and purity are not high, and the performance of dispersed aspect is bad, therefore, inevitably can in film, cause " fog ", directly caused the transparency of system not good.Meanwhile, because natural mineral matter is " heavy " structure, concerning the opening agent of identical weight, effectively particulate sum is few.
Current transparency in the world, the particle type opening agent that opening usefulness is the highest are the synthetic silicides of lightweight.Because it has light structures, therefore, the in the situation that of identical weight, particulate sum is many more than all kinds of heavy natural mineral.Therefore, effective vent composition is far above all kinds of natural mineral.But because the synthetic silicide of lightweight of high-quality has very large specific surface area, manufacture high dispersive opening agent masterbatch, need higher technology and advanced equipment.Much blown film factory brings into use highly purified opening agent now, and its advantage is addition little (0.1%～0.3%), does not affect the transparency of film, is conducive to improve the luminance brightness of film surface, slickness.
The film opening agent extensively adopting is at present mainly the silicon-dioxide that vapor phase process is produced; its production process need to be used oxyhydrogen flame; under the high temperature of 1400 ℃, be hydrolyzed; can produce a large amount of hydrogen chloride gas simultaneously; corrodibility is strong; higher for the requirement of equipment and the requirement of environment protection, production cost is higher.
Summary of the invention
The object of this invention is to provide that a kind of production cost is low, products obtained therefrom purity is high, epigranular, the preparation method of dispersed good microparticle type silica gel thin film opening agent.
For reaching above-mentioned purpose, the present invention has adopted following technical scheme:
A kind of preparation method of microparticle type silica gel thin film opening agent, key step comprises: quantitative sodium silicate aqueous solution is added in reactor, under initial reaction temperature, add inorganic acid solution reaction, regulate pH value to A, after gel, continuing to add inorganic acid solution regulates pH value to B, again through ageing, filter, washing, dry, pulverize postprocessing working procedures, obtain the finished product, wherein, after filtration, first use deionized water wash, until the pH value 6～7 of washing water, add again volatile weak acid to regulate slurry pH value to 4～5, then add wherein the surface tension control agent that accounts for gained silicon-dioxide quality 0.2-0.9%, stir after 5～10 minutes and spray again and be dried, surface tension control agent used is non-ionic type silane dispersion agent or organo silane coupling agent.
The preparation method of described microparticle type silica gel thin film opening agent wherein, adds quantitative sodium silicate solution in reactor during reaction under whipped state, initial reaction temperature is at 20-40 ℃, in reactor, add inorganic acid solution, to forming gel, stirring reaction 1 hour; Then secondary adds inorganic acid solution, adjusts pH value to 3～5; Reheat to 50～60 ℃, add ammoniacal liquor or sodium hydroxide to regulate pH value to 9～10; Then suspension is warming up to 80-100 ℃, ageing 0.5～4 hour; Add again inorganic acid solution to regulate pH value to 2-3, after ageing 3-10 hour, filter, wash and be dried to obtain the finished product.
The preparation method of described microparticle type silica gel thin film opening agent, wherein, the mass ratio of described sodium silicate aqueous solution is 10-20%, modulus 3.2-3.5, iron level is lower than 100ppm; Described inorganic acid solution is that mass ratio is sulfuric acid, hydrochloric acid or the aqueous nitric acid of 25-35%.
The preparation method of described microparticle type silica gel thin film opening agent, the technical indicator of the silicon-dioxide that it obtains is:
Silicon-dioxide contents on dry basis >=99.0%;
Weight loss on heating≤3.5%;
DBP absorption value 1.5～2.5g/g;
Median size
3～4 μ m.
The present invention adds surface tension control agent before spraying is dry, make silica particles silicon hydroxy combining active strong group, reaction generates siloxanes, greatly improve the affine degree of silica dioxide granule and organic polymer, by the redrying technique before packing, reduce weight loss on heating, reduced static.Technique is simple, and raw materials cost is low, and products obtained therefrom purity is high, and particle diameter is little, stable performance.Be applicable to production and the use of high-grade film.
Embodiment
A preparation method for microparticle type silica gel thin film opening agent, it comprises the steps:
(1) raw material
Sodium silicate solution: mass ratio is 10-20%, pure water configuration, modulus 3.2-3.5, iron level is lower than 100ppm;
Inorganic acid solution: mass ratio is 25-35%, can adopt sulfuric acid, hydrochloric acid or nitric acid;
Surface tension control agent: non-ionic type silane dispersant A 1230 or organo silane coupling agent A1810 that MOMENTIVE company produces.
(2) reaction
Under whipped state, quantitative sodium silicate solution is added in reactor, under 20-40 ℃ of condition, add inorganic acid solution, form after gel, keep stirring, continue to add inorganic acid solution, keep stirring 1 hour, whipping process is adjusted in pH value 3～5 scopes; Then be heated to 50～60 ℃, add ammoniacal liquor or sodium hydroxide to regulate pH value to 9～10; Again suspension is warming up to 80-100 ℃, ageing 0.5～4 hour; Add again sulphuric acid soln to regulate pH value for 2-3, ageing 3-10 hour;
(3) filter, wash, be dried
Filter and with deionized water wash to pH value 6～7, the weak acid of easy volatile is as second acid for adjusting pH value 4～5, then in slurry, add the surface tension control agent that accounts for gained silicon-dioxide quality 0.2-0.9%, stir spraying in 5～10 minutes and be dried, comminution by gas stream is processed into finished product.
Embodiment 1
The sodium silicate solution that is 13% by 2000mL mass ratio adds in reactor, adds 30% sulphuric acid soln at 20-40 ℃, forms after gel, adding sulphuric acid soln to be adjusted to pH value is 4, is heated to 60 ℃, and adding ammoniacal liquor to regulate pH value is 10, be warming up to 100 ℃, aging 3 hours; Adding sulphuric acid soln to regulate pH value is 3, ageing 3 hours; Filter and be 7 by deionized water wash to pH value, specific conductivity 26 μ S/cm, 880 grams of the aqueous silica suspension obtaining, according to HG/T3065-2008, measuring its solid content is 25%, in slurry, adding second acid for adjusting pH value is 4, to the organo silane coupling agent A1810 that adds in slurry 1.1Ke MOMENTIVE company to produce as surface tension control agent, stir spraying in 10 minutes dry, comminution by gas stream processed finished products, and by packing after XSJ-150 type spiral-flow flashing drier redrying, obtaining 200 grams of its finished products, is A.
Embodiment 2
Method by embodiment 1 narration is prepared microparticle type silica gel thin film opening agent, as different from Example 1: add the tensio-active agent of 1.8 grams, the organo silane coupling agent A1810 that tensio-active agent adopts MOMENTIVE company to produce, obtains 200 grams of finished products, is B.
Embodiment 3
Method by embodiment 1 narration is prepared microparticle type silica gel thin film opening agent, as different from Example 1: the tensio-active agent that adds 0.44 gram, the non-ionic type silane coupling A 1230 that tensio-active agent adopts MOMENTIVE company to produce, obtains 200 grams of finished products, is C.
Example 4(comparative example 1)
The sodium silicate solution that is 13% by 2000mL mass ratio adds in reactor, adds 30% sulphuric acid soln, forms after gel, and adding sulphuric acid soln to be adjusted to pH value is 4, is heated to 60 ℃, and adding ammoniacal liquor to regulate pH value is 10, is warming up to 100 ℃, aging 3 hours; Adding sulphuric acid soln to regulate pH value is 3, and ageing 3 hours is filtered, and washs to specific conductivity 33 μ S/cm, after spraying is dry, is crushed into finished product, obtains 220 grams of finished products, is D.
Example 5(comparative example 2)
Method by embodiment 2 narrations is prepared microparticle type silica gel thin film opening agent, as different from Example 2: functional quality adds in reactor than the sodium silicate solution that is 10%, adds 35% sulphuric acid soln, obtains 150 grams of finished products, is E.
Test its effect:
After 50mL industrial white oil is mixed with 50kg pp material, by 0.1% additive opening agent of pp material mass ratio (agent of embodiment 1-5 split shed is designated respectively A, B, C, D, E), import W.R.Grace company is used to silicate is raw material simultaneously, (this product is wider in the Application Areas in film field as film opening agent for the Sylobloc45 opening agent product of producing, but expensive, in addition, it is acid that this product pH value is) be designated F, jointly compare.
Use equipment:
High-speed mixer GH-100DL
Parallel equidirectional two-screw forcing machine TE65
Inflation film manufacturing machine SJ45-25L
Test set:
Friction coefficient instrument FMX-1
Stretching strength determination instrument XLW
Photoelectricity haze meter WGW
Laser fineness gage JL1166
Grossmeters MN268
Comparing result in form finds out, silica gel thin film opening agent of the present invention is applied in polypropylene film, and tensile strength, transmittance and mist degree all more existing opening agent increase; Frictional coefficient significantly reduces, and opening performance is obtained and improve; Weight loss on heating is lower, has reduced static, flatting efficiency is better, and product purity is high, and particle diameter is little, stable performance, and product is neutral.
The above, be only preferred embodiment of the present invention, not the present invention done to any pro forma restriction.Any change being equal to, modification or differentiation etc. that all those skilled in the art utilize technical scheme of the present invention to make above-described embodiment, all still belong in the scope of technical solution of the present invention.
Claims (3)
1. the preparation method of a microparticle type silica gel thin film opening agent, key step comprises: under whipped state, quantitative sodium silicate solution is added in reactor, initial reaction temperature adds inorganic acid solution in 20-40 ℃ of downhill reaction still, to forming gel, and stirring reaction 1 hour; Then secondary adds inorganic acid solution, adjusts pH value to 3～5; Reheat to 50～60 ℃, add ammoniacal liquor or sodium hydroxide to regulate pH value to 9～10, then through ageing, filtration, washing, dry, pulverizing postprocessing working procedures, obtain the finished product, it is characterized in that:
After filtration, first use deionized water wash until the pH value 6～7 of washing water, add again volatile weak acid to regulate slurry pH value to 4～5, then add wherein the surface tension control agent that accounts for gained silicon-dioxide quality 0.2-0.9%, stir after 5～10 minutes and spray and be dried, surface tension control agent used is non-ionic type silane dispersion agent or organo silane coupling agent.
2. the preparation method of microparticle type silica gel thin film opening agent according to claim 1, is characterized in that:
Described aging step is: after regulating pH value to 9～10, suspension is warming up to 80-100 ℃, ageing 0.5～4 hour; Add again inorganic acid solution to regulate pH value to 2-3, ageing 3-10 hour.
3. the preparation method of microparticle type silica gel thin film opening agent according to claim 1, is characterized in that:
The mass percent of described sodium silicate solution is 10-20%, modulus 3.2-3.5, and iron level is lower than 100ppm; Described inorganic acid solution is that mass percent is sulfuric acid, hydrochloric acid or the aqueous nitric acid of 25-35%.
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| CN201010611813.6A CN102532950B (en) | 2010-12-17 | 2010-12-17 | Preparation method for microparticle type silica gel thin film opening agent |
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| CN201010611813.6A CN102532950B (en) | 2010-12-17 | 2010-12-17 | Preparation method for microparticle type silica gel thin film opening agent |
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| CN102532950B true CN102532950B (en) | 2014-03-12 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102827495A (en) * | 2012-09-17 | 2012-12-19 | 福建省三明同晟化工有限公司 | Preparation method of high transparent precipitated silica for plastic anti-block agent |
| CN103360796A (en) * | 2013-06-25 | 2013-10-23 | 安徽敬业纳米科技有限公司 | Method for in situ modification of amphoteric nano silica |
| CN106750749B (en) * | 2016-11-30 | 2020-11-10 | 黄山贝诺科技有限公司 | Silicon dioxide-based opening agent for polyolefin film and preparation method thereof |
| CN106752275A (en) * | 2017-01-11 | 2017-05-31 | 冷水江三A新材料科技有限公司 | A kind of preparation method of elastic handfeel paint Coating Matting powder |
| CN111094184A (en) * | 2017-08-31 | 2020-05-01 | 株式会社德山 | Surface-treated sol-gel silica and method for producing same |
| CN109705402B (en) * | 2019-01-08 | 2020-07-10 | 广州凌玮科技股份有限公司 | Preparation method of aerogel film opening 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 |
| CN116004036A (en) * | 2022-11-25 | 2023-04-25 | 冷水江三A新材料科技有限公司 | Preparation method of sol-gel method film opening agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1896000A (en) * | 2003-02-21 | 2007-01-17 | 青岛海洋化工有限公司 | Production of macroporous silica gel |
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| KR100848856B1 (en) * | 2007-03-27 | 2008-07-29 | 주식회사 넵 | Method for preparing hydrophobic surface aerogel and hydrophobic surface aerogel therefrom |
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| CN1896000A (en) * | 2003-02-21 | 2007-01-17 | 青岛海洋化工有限公司 | Production of macroporous silica gel |
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Granted publication date: 20140312 Termination date: 20211217 |