CN100395183C - Method for preparing high modulus water-soluble potassium silicate and its use for wood processing - Google Patents
Method for preparing high modulus water-soluble potassium silicate and its use for wood processing Download PDFInfo
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- CN100395183C CN100395183C CNB2006100357550A CN200610035755A CN100395183C CN 100395183 C CN100395183 C CN 100395183C CN B2006100357550 A CNB2006100357550 A CN B2006100357550A CN 200610035755 A CN200610035755 A CN 200610035755A CN 100395183 C CN100395183 C CN 100395183C
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- potassium silicate
- water
- soluble potassium
- high modulus
- modulus water
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Abstract
The present invention relates to a method for preparing high modulus water soluble potassium silicate and application for wood processing thereof. The method comprises following steps: (1) hydrating lithium hydroxide and deionized water are added into a stainless steel reaction kettle; (2) a jacket of the reaction kettle is led with steam or hot water under a stirring condition, and the temperature rises to 85 DEG C; (3) silicon dioxide is added in two times; (4) after the last part of the silicon dioxide is added, the temperature rises to 95 DEG C; 5) when the viscosity of the material in the kettle is reduced, samples is taken for detecting solid portion, the loss of water caused by evaporation is supplied, the specified solid portion is regulated, and a product leaves the reaction kettle. The adhesive is used for the manufacture of inorganic paint and fireproofing material and is also used in wood processing. The wood products processed by the product have a fire proofing, a moisture proofing, a decay preventing and a termite resisting effects. When the present invention is used for the adhesion of wood, indoor air pollution and harm for the human body caused by the formaldehyde of formaldehyde resin can be thoroughly eliminated.
Description
Technical field:
The present invention relates to the manufacture method and the applied technical field thereof of water-soluble potassium silicate, particularly the manufacture method of high modulus water-soluble potassium silicate and the application in wood working thereof.
Background technology:
Research to mineral binder bond can be traced back to the fifties in last century the earliest.To the sixties and the seventies, because the influence of oil crisis, the chemist has given very big concern to the synthetic and application of inorganic adhesive.At that time, many research report and patent applications about inorganic adhesive preparation method and application had abroad appearred.Except cement, mineral binder bond mainly contains two kinds: 1, water-soluble alkali metal silicates and silicon sol; 2, water-soluble condensation phosphoric acid salt.The water-soluble alkali metal silicates mineral binder bond is used more, is mainly used in building coating, protective system, high-temperature resistant coating and refractory materials.It is few that water-soluble condensation phosphate binders is used, and is mainly used in refractory materials, for example high temperature furnace lining etc.
The water-soluble alkali metal silicates binding agent is the water-dilutable product, have nontoxic, pollution-free, do not fire and characteristics such as high temperature resistant.Simultaneously, it has been completely free of the dependence to petroleum resources.Research for manufacture method, performance and the application of this binding agent never stopped, and had also obtained some progress.According to report, a kind of alkalimetal silicate mineral binder bond of excellent property should have good curing performance and adhesive property, and good water tolerance and weather resistance are arranged after curing.For this reason, should reduce alkali-metal content as far as possible, high modulus (SiO promptly will be arranged
2/ Me
2The ratio of the molecule number of O, Me
2O is an alkalimetal oxide).In addition, in order to guarantee this binding agent good stability is arranged, its water-soluble inorganic salts contg should be low as far as possible.
More as can be known, high-module (4.5～10) water-soluble potassium silicate is best a kind of of performance from three kinds of available water-soluble alkali metal silicates binding agent performances.But, can not produce high modulus water-soluble potassium silicate with traditional dry method (roasting method), can only adopt wet method (leaching method) to produce.The chemical engineer is to having done many research work with the wet production high modulus water-soluble potassium silicate, and the high modulus water-soluble potassium silicate of super quality and competitive price is produced in attempt with simple method.Relevant patent report comes across 1954 the earliest, and this patent proposes a kind of method for preparing high modulus water-soluble potassium silicate.This method is the silicon sol process ion exchange resin treatment that commercially available alkali (NaOH or KOH) is stable, removes sodium or potassium ion and other water-soluble impurity; After this, add lithium hydroxide solution, stir, pass through the slaking of room temperature peptization again, make modulus and be 4～25 lithium silicate solution.Occurred several parts of patent reports in 1964 in the period of to 1970, wherein had two parts of patents also to propose to produce with silicon sol and lithium hydroxide the method for high modulus water-soluble potassium silicate, the method in they and the first part of patent is similar.Other two parts of patents then propose to prepare with silica gel and lithium hydroxide the method for high modulus water-soluble potassium silicate.This method need be in the reaction down of pressurization (70 pounds/square inch) and high temperature (150 ℃), or in heating (80～100 ℃) with leach while hot in the complex techniques process that precipitates product and make product.
The high modulus water-soluble potassium silicate binding agent has good curing performance, resistance toheat, water repelling property, weather resistance and organic solvent resistance, and its application prospect is very wide.Therefore, the method for seeking a kind of simple, cheap manufacturing high modulus water-soluble potassium silicate is of great practical significance.
Summary of the invention:
The objective of the invention is to provide at the deficiencies in the prior art a kind of manufacture method of new high modulus water-soluble potassium silicate and the application in wood working thereof, its modulus can reach between 4.5～10.
For achieving the above object, the present invention adopts following technical scheme: the manufacture method of high modulus water-soluble potassium silicate, and it comprises the following steps: (1), hydronium(ion) oxidation lithium and deionized water is added in the stainless steel cauldron; (2), under agitation, chuck feeding steam or hot water through reactor heat to 85 ℃; (3), gradation adds silicon-dioxide; (4), after adding last batch of silicon-dioxide, be warmed up to 95 ℃; (5), when treating that material viscosity diminishes in the still, sampling and measuring solid part is added the moisture that reduces because of vaporization losses, adjusts to solid part of regulation, can take the dish out of the pot.
Wherein, divide four times and add silicon-dioxide.
All needed insulation reaction about 2 hours after each the feeding in raw material, treat to add next batch silicon-dioxide after denseness reduces.
In (2) step, intensification and holding temperature are at 85 ± 2 ℃.
In (4) step, heat up and maintain 95 ± 2 ℃, reacted about 3 hours.
In high modulus water-soluble potassium silicate, add organosilane monomer, the mass percent of the organosilane monomer of adding be solid content be 30% water-soluble potassium silicate total amount 1～5%.
In high modulus water-soluble potassium silicate, add subsidiary material, wherein, the volume percent of the emulsion-type binding agent that adds is 20～40% of a mixed glue solution, the volume percent of the stopping composition that adds is 15～60% of a mixed glue solution, and the volume percent of the curing catalyst of adding accounts for 1～5% of mixed glue solution.
The water-soluble potassium silicate binding agent of the inventive method manufacturing can reach the optimal modulus scope, and promptly 4.5～10; In addition, the water-soluble potassium silicate binding agent can be used in woodwork processing, with the woodwork that this product treatment is crossed, has fire prevention, protection against the tide, anti-rotting and termite-proof effect, when being used for wood bonding, can thoroughly eliminate formaldehyde that three-aldehyde glue causes to the pollution of room air with to the harm of human body.
Embodiment:
Main purpose of the present invention is the manufacture method that proposes a kind of simple, cheap high modulus water-soluble potassium silicate.
(1) hydronium(ion) oxidation lithium and deionized water are added in the stainless steel cauldron; (2) under agitation, chuck feeding steam or hot water through reactor heat to 85 ℃, and holding temperature is at 85 ± 2 ℃; (3) divide four times and add silicon-dioxide, all needed insulation reaction about 2 hours after each the feeding in raw material; (4) treat to add next batch silicon-dioxide after denseness reduces; After adding last batch of silicon-dioxide, be warmed up to 95 ℃, keep about 3 hours of reaction at 95 ± 2 ℃; When (5) treating that material viscosity diminishes in the still, sampling and measuring solid part is added the moisture that reduces because of vaporization losses, adjusts to solid part of regulation, can take the dish out of the pot.
Reactor should be equipped with reflux exchanger, reduces moisture loss as far as possible.
The main raw material that present method adopts is: (1) active SiO
2Material: precipitated silica, thermal silica, finely divided silica gel and as other active silica of chemical industry by product; (2) industrial hydration lithium hydroxide (LiOHH
2O); (3) deionized water.
Another object of the present invention is to propose the optimal modulus scope of water-soluble potassium silicate binding agent.In this optimum range (4.5～10), the water-soluble potassium silicate binding agent shows best package stability, good curing performance and physical and mechanical properties and good water-fast and corrosion resistance.The SiO of water-soluble potassium silicate binding agent
2Content is between 20～25%, and it is suitable for the various uses and the constructional method of water-soluble potassium silicate.
Another object of the present invention is the method for modifying that proposes the high modulus water-soluble potassium silicate binding agent.In order to adapt to some particular requirements of different purposes, need in the water-soluble potassium silicate binding agent, add some organosilane monomers as properties-correcting agent; For example, trimethoxymethylsila,e, dimethoxy dimethylsilane, di ethoxy di methyl-monosilane, methyl silicon sodium alcoholate and some coupling agent etc.The mass percent of the organosilane monomer that adds be solid content be 30% water-soluble potassium silicate total amount 1～5%.These properties-correcting agent can improve the toughness of the processing of glue and package stability, raising glue-line and hydrophobicity and to the moisture dispersibility of color stuffing.
Another object of the present invention is that the high modulus water-soluble potassium silicate binding agent is applied in the wood processing field.Under same modulus, lithium silicate is compared with water glass or potassium silicate, and alkaline matter content is minimum, and water insoluble basically owing to lithium silicate after curing, so it can be used, the effect of quickening decay of wood can not arranged as water glass and potassium silicate in wood working.Timber with the high modulus water-soluble potassium silicate solution impregnation does not at high temperature burn, and only therefore the meeting dehydration carbonization can make timber have fire retardant performance.High modulus water-soluble potassium silicate cementing layer after the curing has good water tolerance, so it gives good protection against the tide of timber and water resistance; Thereby can prevent decay of wood.In addition, once find to prevent effectively the infringement of termite with the timber that this product treatment is crossed.In the processing of the bonding of timber, use formaldehyde that the high modulus water-soluble potassium silicate tackiness agent can thoroughly eliminate three-aldehyde glue (urine aldehyde glue, phenolic glue and melamino-formaldehyde glue) to the pollution of indoor environment with to the harm of human body.This product can be used with various emulsion-type binding agents (benzene emulsion, PVA emulsion, VAE emulsion, pure-acrylic emulsion and latex powder etc.) amalgamation when being used for wood bonding, and the volume percent of the emulsion-type binding agent of adding is 20～40% of a mixed glue solution.In addition, can add various stopping composition, for example: kaolin, wollastonite, lime carbonate, talcum powder, diatomite and silica powder etc., the volume percent of the stopping composition of adding is 15～60% of a mixed glue solution.In order to quicken the curing of glue-line, when joining glue, can add curing catalyst, for example: borax, zinc oxide, Repone K, Potassium Bromide, zinc borate, lime borate etc., the volume percent of the curing catalyst of adding accounts for 1～5% of mixed glue solution.
Technical scheme of the present invention can be done by following specific embodiment and explain:
Embodiment 1:
With 65 kilograms of deionized waters and hydronium(ion) oxidation lithium (LiOHH
2O) in 7.7 kilograms of adding reactors, heat to 85 ℃, insulation and under agitation divides four times and adds 27.3 kilograms of precipitated silicas, all needs insulation reaction 2 hours after reinforced at every turn, treats that the material denseness reduces back adding next batch material.After adding the last batch of material, be warmed up to 95 ℃ of insulation reaction 3 hours.After this, measure solids constituent, add the water of vaporization losses, get final product discharging.This product modulus 4.46, solid is divided into 28.5%.
Embodiment 2:
Prescription: 66.1 kilograms of deionized waters, 6.8 kilograms of hydronium(ion) oxidation lithiums, 27.1 kilograms in finely divided silica gel.
Technology: with embodiment 1
Product modulus 5.0, solid is divided into 28.5%
Embodiment 3, the method for modifying of high modulus water-soluble potassium silicate binding agent:
Prescription: 62.8 kilograms of deionized waters, 6.45 kilograms of hydronium(ion) oxidation lithiums, 30.75 kilograms of gas-phase silicas, 2 kilograms of di ethoxy di methyl-monosilanes.
Technology: with embodiment 1.After last holding stage finishes, cool to 60 ℃, in 1 hour, be added dropwise to di ethoxy di methyl-monosilane.After this, measure solids constituent, add the water of vaporization losses, get final product discharging.This product modulus is 6.3, and solid is divided into 32%.
Embodiment 4:
When this product is used for the woodwork bonding, join glue embodiment.
Lithium silicate solution (30%) 100
Benzene emulsion (50%) 18
Calucium Silicate powder (325 order) 30
Zinc oxide 3
Using on-the-spot preparation, used up the same day.But pressurized, heated is quickened to solidify.
Claims (7)
1. the manufacture method of high modulus water-soluble potassium silicate, it is characterized in that: it comprises the following steps:
(1), hydronium(ion) oxidation lithium and deionized water are added in the stainless steel cauldron;
(2), under agitation, chuck feeding steam or hot water through reactor heat to 85 ℃;
(3), gradation adds silicon-dioxide;
(4), after adding last batch of silicon-dioxide, be warmed up to 95 ℃;
(5), when treating that material viscosity diminishes in the still, sampling and measuring solid part is added the moisture that reduces because of vaporization losses, adjusts to solid part of regulation, can take the dish out of the pot.
2. the manufacture method of high modulus water-soluble potassium silicate according to claim 1 is characterized in that: divide four times and add silicon-dioxide.
3. the manufacture method of high modulus water-soluble potassium silicate according to claim 1 and 2 is characterized in that: all needed insulation reaction about 2 hours after each the feeding in raw material, treat can add next batch silicon-dioxide after denseness reduces.
4. the manufacture method of high modulus water-soluble potassium silicate according to claim 1 is characterized in that: in (2) step, heat up and holding temperature at 85 ± 2 ℃.
5. the manufacture method of high modulus water-soluble potassium silicate according to claim 1 is characterized in that: in (4) step, heat up and maintain 95 ± 2 ℃, reacted about 3 hours.
6. the manufacture method of high modulus water-soluble potassium silicate according to claim 1, it is characterized in that: in high modulus water-soluble potassium silicate, add organosilane monomer, the mass percent of the organosilane monomer of adding be solid content be 30% water-soluble potassium silicate total amount 1～5%.
7. the application of high modulus water-soluble potassium silicate in wood working, it is characterized in that: in high modulus water-soluble potassium silicate, add subsidiary material, wherein, the volume percent of the emulsion-type binding agent that adds is 20～40% of a mixed glue solution, the volume percent of the stopping composition that adds is 15～60% of a mixed glue solution, and the volume percent of the curing catalyst of adding accounts for 1～5% of mixed glue solution.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100357550A CN100395183C (en) | 2006-06-02 | 2006-06-02 | Method for preparing high modulus water-soluble potassium silicate and its use for wood processing |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100357550A CN100395183C (en) | 2006-06-02 | 2006-06-02 | Method for preparing high modulus water-soluble potassium silicate and its use for wood processing |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1850601A CN1850601A (en) | 2006-10-25 |
| CN100395183C true CN100395183C (en) | 2008-06-18 |
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|---|---|---|---|
| CNB2006100357550A Expired - Fee Related CN100395183C (en) | 2006-06-02 | 2006-06-02 | Method for preparing high modulus water-soluble potassium silicate and its use for wood processing |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103305129A (en) * | 2013-05-30 | 2013-09-18 | 玖青涂料（上海）有限公司 | Modified inorganic lithium silicate binder, and preparation method and use thereof |
| CN103265045A (en) * | 2013-06-03 | 2013-08-28 | 田辉明 | Method for producing potassium silicate solution for electronic industry |
| CN103773253B (en) * | 2014-01-17 | 2015-09-23 | 中南林业科技大学 | A kind of fire-resistant waterproof silicate based Wood Adhesives and preparation method thereof |
| CN110948625A (en) * | 2019-11-29 | 2020-04-03 | 大亚人造板集团有限公司 | Waterproof agent for artificial board and application process thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1183120A (en) * | 1966-11-30 | 1970-03-04 | Henkel & Cie Gmbh | A Process for the Preparation of Lithium Silicate Solutions |
| GB1198313A (en) * | 1966-11-08 | 1970-07-08 | Philadelphia Quartz Co | Manufacture of Lithium Silicate Solutions |
| JPS5420480A (en) * | 1977-07-15 | 1979-02-15 | Toshiba Corp | Device for clamping gasket |
| JPS5969417A (en) * | 1982-10-08 | 1984-04-19 | Nippon Chem Ind Co Ltd:The | Manufacture of lithium silicate |
| GB2159807A (en) * | 1984-04-25 | 1985-12-11 | Kernforschungsz Karlsruhe | Method of producing a sinterable lithium metasilicate Li2SiO3 powder |
| JP2000313615A (en) * | 1999-04-28 | 2000-11-14 | Nippon Chem Ind Co Ltd | Production of lithium silicate |
-
2006
- 2006-06-02 CN CNB2006100357550A patent/CN100395183C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1198313A (en) * | 1966-11-08 | 1970-07-08 | Philadelphia Quartz Co | Manufacture of Lithium Silicate Solutions |
| GB1183120A (en) * | 1966-11-30 | 1970-03-04 | Henkel & Cie Gmbh | A Process for the Preparation of Lithium Silicate Solutions |
| JPS5420480A (en) * | 1977-07-15 | 1979-02-15 | Toshiba Corp | Device for clamping gasket |
| JPS5969417A (en) * | 1982-10-08 | 1984-04-19 | Nippon Chem Ind Co Ltd:The | Manufacture of lithium silicate |
| GB2159807A (en) * | 1984-04-25 | 1985-12-11 | Kernforschungsz Karlsruhe | Method of producing a sinterable lithium metasilicate Li2SiO3 powder |
| JP2000313615A (en) * | 1999-04-28 | 2000-11-14 | Nippon Chem Ind Co Ltd | Production of lithium silicate |
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| CN1850601A (en) | 2006-10-25 |
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