CN107090250A - A kind of method for preparing industrial metasilicate adhesive - Google Patents
A kind of method for preparing industrial metasilicate adhesive Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J1/00—Adhesives based on inorganic constituents
- C09J1/02—Adhesives based on inorganic constituents containing water-soluble alkali silicates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/262—Alkali metal carbonates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/50—Phosphorus bound to carbon only
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L29/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
- C08L29/02—Homopolymers or copolymers of unsaturated alcohols
- C08L29/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L3/00—Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
- C08L3/04—Starch derivatives, e.g. crosslinked derivatives
- C08L3/06—Esters
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- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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Abstract
A kind of method for preparing industrial metasilicate adhesive, first prepare sodium orthosilicate crude product, sodium silicate solid is prepared again, the sodium silicate solid is dissolved in special adhesive and water mixed solution, then filter, sodium silicate solution is obtained, sodium hydrogensulfite generation precipitated silica and sodium sulfite solution are added in the sodium silicate solution, the mixture of generation is filtered；Another part filtrate of filtrate is concentrated and dried, and obtains high-quality industrial metasilicate；The high-quality industrial metasilicate of preparation is mixed with 2 times of resin emulsion, is added in silica sand, is sufficiently mixed and produces waterglass adhesive.Main component after waterglass hardening is Silica hydrogel and solid, specific surface area is big, greatly improve cohesive force, waterglass is handled using the special adhesive and water mixed solution of intermediate concentration, improve water resistance, transport, store and very easy to use, be particularly suitable for use in mechanization, automation mechanized operation.
Description
Technical field：
The present invention relates to chemical field, and in particular to a kind of method for preparing industrial metasilicate adhesive.
Background technology：
Sodium metasilicate is commonly called as sodium silicate, is a kind of water-soluble silicate, and its aqueous solution is commonly called as waterglass, is a kind of ore deposit bonding
Agent.Its chemical formula is R2OnSiO2, and R2O is alkali metal oxide in formula, and n is silica and alkali metal oxide molal quantity
Ratio, referred to as waterglass the number that rubs.Architectural conventional waterglass is sodium metasilicate (Na2OnSiO2) aqueous solution.
The purposes of waterglass widely, almost throughout each department of national economy.Manufacture is used in chemical system
Silica gel, white carbon, zeolite molecular sieve, metasilicate pentahydrate sodium, Ludox, layer silicon and instant powdery sodium silicate, sodium potassium silicate etc. are each
Silicates product is planted, is the base stock of silicon compound.In developed country, using sodium metasilicate as the deep processing of raw material series
Product has developed to more than 50 kinds, and some are applied to high, precision and frontier sciemtifec and technical sphere；It is the washing such as washing powder, soap in light industry
Indispensable raw material in agent, is also water softener, settling agent；It is used for assisting-dyeing, bleaching and sizing in textile industry；In machine
Casting, emery wheel manufacture and anticolodal etc. are widely used in tool industry；In building trade be used for manufacture quick hardening cement, it is acidproof
Cement water-proof oil, soil-solidified-agent, refractory material etc.；Silicon element fertilizer material can agriculturally be manufactured；Oil catalysis is additionally may act as to split
Exotic material, anticolodal, the water such as the silica-alumina catalyst of change, the filler of soap, the adhesive of corrugated paper, laboratory crucibles
Softening agent, detergent builders, refractory material and ceramic raw material, the drift of textile, dye and slurry, mine ore dressing, waterproof, leak stopping,
Fire retarding wood protection, food antiseptic and preparing adhesive etc..
Main component after waterglass hardening is Silica hydrogel and solid, and specific surface area is big, thus with higher cohesive force.
But waterglass sole mass, batch performance and construction and maintenance have a significant impact to intensity.
The content of the invention：
The technical problems to be solved by the invention are that overcoming prior art to provide one kind prepares industrial metasilicate adhesive
Method.
The technical problems to be solved by the invention are realized using following technical scheme.
A kind of method for preparing industrial metasilicate adhesive, it is characterised in that：Comprise the following steps and be prepared from：
1) solid sodium hydroxide and silicon powder are compared into 2.5-3 according to weight:1 ratio is added in electric smelter, heating curve
200 DEG C are warming up to according to 8-10 DEG C/min, then 320-350 DEG C is warming up to according to 4-6 DEG C/min, made after heating described
Solid sodium hydroxide is melted, and is further continued for being warming up to 400-450 DEG C according to 4-6 DEG C/min, is stopped heating, until the silicon powder
Reaction is complete, produces sodium orthosilicate crude product；
2) environment temperature where sodium orthosilicate crude product is increased to 100 DEG C~140 DEG C, is incubated 0.5~1 hour；Temperature liter
Up to 190 DEG C~210 DEG C, it is incubated 1~2 hour；Temperature is increased to 295 DEG C~305 DEG C, is incubated 1.8~2.5 hours；Again by institute
State sodium orthosilicate crude product and be cooled to less than 40 DEG C, make the sodium orthosilicate crude product completion of cure, produce sodium silicate solid；
3) sodium silicate solid is dissolved in water, then filtered, obtain sodium silicate solution, added in the sodium silicate solution
Enter sodium hydrogensulfite generation precipitated silica and sodium sulfite solution, the mixture of generation is filtered；
4) by a part for the filtrate produced at the end of step (3) and the sulfur dioxide haptoreaction, and the Asia of generation
Niter cake product is recycled to recycling in step (3)；
5) filter cake obtained at the end of step (3) is acidified, be filtered, washed and dried, obtain light silicon dioxide；
6) another part filtrate of the filtrate produced at the end of step (3) is concentrated and dried, obtains high-quality industrial silicon
Sour sodium；
7) the high-quality industrial metasilicate of preparation is mixed with 2 times of resin emulsion, special adhesive is put into after mixing
In water mixed solution, during, the water-gas produced using gas generator passes sequentially through cyclone dust collectors, exchanger and storage
Hot cell, regenerator is provided with interlayer, the waste heat pipe connection of interlayer and gas generator, by the waste heat of gas generator to mixing
Solution is incubated, and stirs homogeneous, stirring duration 3 minutes, stops insulation, and natural cooling, precipitation removes moisture removal, by sediment
After drying, add in silica sand, be sufficiently mixed and produce waterglass adhesive.
Further technology：Described adhesive and water mixed solution is prepared from including following components：Ester solidifies waterglass
10-13 parts of self-hardening sand, phosphate ester starch -101-130 parts of natural plant gum copolymerization adhesive, 65-80 parts of fiber, 2-5 parts of ammonium persulfate,
3-5 parts of polyvinyl alcohol, 1-20 parts of sodium carbonate, 450-500 parts of hydrogen peroxide, 45-50 parts of dimethyl silicone rubber, 1-2 parts of absolute ethyl alcohol,
10-15 parts of silica particles, 20% 15-20 parts of aqueous sodium carbonate, calcium hydroxide:10-20 parts, 2300-2600 parts of water, triphen
2-5 parts of base phosphorus, 20-27 parts of chloride hydrate rhodium, 13-16 parts of catalyst, 200-220 parts of natural plant gum.
Further technology：Described adhesive and water mixed solution is prepared from including following components：Ester solidifies waterglass
10 parts of self-hardening sand, phosphate ester starch -101 parts of natural plant gum copolymerization adhesive, 65 parts of fiber, 2 parts of ammonium persulfate, 3 parts of polyvinyl alcohol,
1 part of sodium carbonate, hydrogen peroxide:450 parts, dimethyl silicone rubber：45 parts, 1 part of absolute ethyl alcohol, 10 parts of silica particles, 20% carbonic acid
15 parts of sodium water solution, 10 parts of calcium hydroxide, 2300 parts of water, 2 parts of triphenyl phosphorus, 20 parts of chloride hydrate rhodium, 13 parts of catalyst, plant
200 parts of glue.
Further technology：Described adhesive and water mixed solution is prepared from including following components：Ester solidifies waterglass
13 parts of self-hardening sand, phosphate ester starch -130 parts of natural plant gum copolymerization adhesive, 80 parts of fiber, 5 parts of ammonium persulfate, 5 parts of polyvinyl alcohol,
20 parts of sodium carbonate, 500 parts of hydrogen peroxide, 50 parts of dimethyl silicone rubber, 2 parts of absolute ethyl alcohol, 15 parts of silica particles, 20% sodium carbonate
20 parts of the aqueous solution, 20 parts of calcium hydroxide, 2600 parts of water, 5 parts of triphenyl phosphorus, 27 parts of chloride hydrate rhodium, 16 parts of catalyst, natural plant gum
220 parts.
Further technology：Described adhesive and water mixed solution are mainly prepared from by following steps：
20% aqueous sodium carbonate is added in phosphate ester starch-natural plant gum copolymerization adhesive, is then stirring and/or is surpassing
It is slowly added to react 0.1~12 hour at a temperature of ammonium persulfate and hydrogen peroxide, 0~80 DEG C under sound effect, after reaction terminates, adds
System pH is adjusted to 7 by sodium carbonate；
Fiber and silica particles are wrapped up with cloth, are put into above-mentioned steps, is distilled, 12-14 minutes, cloth bag is taken out, will
Fiber and white carbon mixing, dry, particle are made；
Take particle to be mixed with calcium hydroxide, add in the round-bottomed flask equipped with reflux condensing tube, add anhydrous after degassing
Ethanol, heating water bath to 90 DEG C of backflows is completely dissolved triphenyl phosphorus, then the hydration chlorine for being dissolved in ethanol is added from condenser pipe upper end
Change rhodium, reaction precipitate is filtered, washed, dried to permanent quality, obtaining catalyst three by nitrogen protection, return stirring reaction 2h
Phenylphosphine radium chloride RhCl (PPh3) 3；
Dimethyl silicone rubber is added in autoclave, catalyst RhCl (PPh3) 3 is added after deaeration, it is warming up to
100 DEG C, be passed through hydrogen to 5.6MPa, reaction discharges after 11 hours, and reaction product inserts 40 DEG C of vacuum after being condensed with isopropanol
72h is dried in baking oven；
It is added to after drying in natural plant gum, stirs, be added to the water.
Beneficial effect：Main component after waterglass hardening is Silica hydrogel and solid, and specific surface area is big, greatly improves bonding
Power, is handled waterglass using the special adhesive and water mixed solution of intermediate concentration, improves water resistance, transport,
Store and very easy to use, be particularly suitable for use in mechanization, automation mechanized operation.It is widely used in metallurgy, electric power, petrochemical industry and building materials
In industry.Compared by the anhydrous powder shape sodium metasilicate of mechanical crushing, this law prepare sodium metasilicate water-soluble speed, purity level all
Be mixed into higher than anhydrous powder shape sodium metasilicate, then by sodium metasilicate in special adhesive and water mixed solution, constantly with water
Adhesive is mixed, and greatly lifts its stick effect.
Modulus of water glass is general between 2.4~3.3.1.36~1.50g/cm of density of conventional waterglass3。
Modulus of water glass is general between 2.7~3.4.1.80~2.11g/cm of density of this law waterglass3, density gets over
Greatly, waterglass content is higher, and viscosity is bigger.
Embodiment：
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment 1：A kind of method for preparing industrial metasilicate adhesive, comprises the following steps and is prepared from：
1) solid sodium hydroxide and silicon powder are compared into 2.5-3 according to weight:1 ratio is added in electric smelter, heating curve
200 DEG C are warming up to according to 8-10 DEG C/min, then 320-350 DEG C is warming up to according to 4-6 DEG C/min, made after heating described
Solid sodium hydroxide is melted, and is further continued for being warming up to 400-450 DEG C according to 4-6 DEG C/min, is stopped heating, until the silicon powder
Reaction is complete, produces sodium orthosilicate crude product；
2) environment temperature where sodium orthosilicate crude product is increased to 100 DEG C~140 DEG C, is incubated 0.5~1 hour；Temperature liter
Up to 190 DEG C~210 DEG C, it is incubated 1~2 hour；Temperature is increased to 295 DEG C~305 DEG C, is incubated 1.8~2.5 hours；Again by institute
State sodium orthosilicate crude product and be cooled to less than 40 DEG C, make the sodium orthosilicate crude product completion of cure, produce sodium silicate solid；
3) sodium silicate solid is dissolved in water, then filtered, obtain sodium silicate solution, added in the sodium silicate solution
Enter sodium hydrogensulfite generation precipitated silica and sodium sulfite solution, the mixture of generation is filtered；
4) by a part for the filtrate produced at the end of step (3) and the sulfur dioxide haptoreaction, and the Asia of generation
Niter cake product is recycled to recycling in step (3)；
5) filter cake obtained at the end of step (3) is acidified, be filtered, washed and dried, obtain light silicon dioxide；
6) another part filtrate of the filtrate produced at the end of step (3) is concentrated and dried, obtains high-quality industrial silicon
Sour sodium；
7) the high-quality industrial metasilicate of preparation is mixed with 2 times of resin emulsion, special adhesive is put into after mixing
In water mixed solution, during, the water-gas produced using gas generator passes sequentially through cyclone dust collectors, exchanger and storage
Hot cell, regenerator is provided with interlayer, the waste heat pipe connection of interlayer and gas generator, by the waste heat of gas generator to mixing
Solution is incubated, and stirs homogeneous, stirring duration 3 minutes, stops insulation, and natural cooling, precipitation removes moisture removal, by sediment
After drying, add in silica sand, be sufficiently mixed and produce waterglass adhesive.
Adhesive and water mixed solution are prepared from including following components：10 parts of self-setting silicate process of ester solidification, phosphate
Starch -101 parts of natural plant gum copolymerization adhesive, 65 parts of fiber, 2 parts of ammonium persulfate, 3 parts of polyvinyl alcohol, 1 part of sodium carbonate, hydrogen peroxide:
450 parts, dimethyl silicone rubber：45 parts, 1 part of absolute ethyl alcohol, 10 parts of silica particles, 20% 15 parts of aqueous sodium carbonate, hydrogen-oxygen
Change 10 parts of calcium, 2300 parts of water, 2 parts of triphenyl phosphorus, 20 parts of chloride hydrate rhodium, 13 parts of catalyst, 200 parts of natural plant gum.
Adhesive and water mixed solution are mainly prepared from by following steps：
20% aqueous sodium carbonate is added in phosphate ester starch-natural plant gum copolymerization adhesive, is then stirring and/or is surpassing
It is slowly added to react 0.1~12 hour at a temperature of ammonium persulfate and hydrogen peroxide, 0~80 DEG C under sound effect, after reaction terminates, adds
System pH is adjusted to 7 by sodium carbonate；
Fiber and silica particles are wrapped up with cloth, are put into above-mentioned steps, is distilled, 12-14 minutes, cloth bag is taken out, will
Fiber and white carbon mixing, dry, particle are made；
Take particle to be mixed with calcium hydroxide, add in the round-bottomed flask equipped with reflux condensing tube, add anhydrous after degassing
Ethanol, heating water bath to 90 DEG C of backflows is completely dissolved triphenyl phosphorus, then the hydration chlorine for being dissolved in ethanol is added from condenser pipe upper end
Change rhodium, reaction precipitate is filtered, washed, dried to permanent quality, obtaining catalyst three by nitrogen protection, return stirring reaction 2h
Phenylphosphine radium chloride RhCl (PPh3) 3；
Dimethyl silicone rubber is added in autoclave, catalyst RhCl (PPh3) 3 is added after deaeration, it is warming up to
100 DEG C, be passed through hydrogen to 5.6MPa, reaction discharges after 11 hours, and reaction product inserts 40 DEG C of vacuum after being condensed with isopropanol
72h is dried in baking oven；
It is added to after drying in natural plant gum, stirs, be added to the water.
Embodiment 2：A kind of method for preparing industrial metasilicate adhesive, comprises the following steps and is prepared from：
1) solid sodium hydroxide and silicon powder are compared into 2.5-3 according to weight:1 ratio is added in electric smelter, heating curve
200 DEG C are warming up to according to 8-10 DEG C/min, then 320-350 DEG C is warming up to according to 4-6 DEG C/min, made after heating described
Solid sodium hydroxide is melted, and is further continued for being warming up to 400-450 DEG C according to 4-6 DEG C/min, is stopped heating, until the silicon powder
Reaction is complete, produces sodium orthosilicate crude product；
2) environment temperature where sodium orthosilicate crude product is increased to 100 DEG C~140 DEG C, is incubated 0.5~1 hour；Temperature liter
Up to 190 DEG C~210 DEG C, it is incubated 1~2 hour；Temperature is increased to 295 DEG C~305 DEG C, is incubated 1.8~2.5 hours；Again by institute
State sodium orthosilicate crude product and be cooled to less than 40 DEG C, make the sodium orthosilicate crude product completion of cure, produce sodium silicate solid；
3) sodium silicate solid is dissolved in water, then filtered, obtain sodium silicate solution, added in the sodium silicate solution
Enter sodium hydrogensulfite generation precipitated silica and sodium sulfite solution, the mixture of generation is filtered；
4) by a part for the filtrate produced at the end of step (3) and the sulfur dioxide haptoreaction, and the Asia of generation
Niter cake product is recycled to recycling in step (3)；
5) filter cake obtained at the end of step (3) is acidified, be filtered, washed and dried, obtain light silicon dioxide；
6) another part filtrate of the filtrate produced at the end of step (3) is concentrated and dried, obtains high-quality industrial silicon
Sour sodium；
7) the high-quality industrial metasilicate of preparation is mixed with 2 times of resin emulsion, special adhesive is put into after mixing
In water mixed solution, during, the water-gas produced using gas generator passes sequentially through cyclone dust collectors, exchanger and storage
Hot cell, regenerator is provided with interlayer, the waste heat pipe connection of interlayer and gas generator, by the waste heat of gas generator to mixing
Solution is incubated, and stirs homogeneous, stirring duration 3 minutes, stops insulation, and natural cooling, precipitation removes moisture removal, by sediment
After drying, add in silica sand, be sufficiently mixed and produce waterglass adhesive.
Adhesive and water mixed solution are prepared from including following components：13 parts of self-setting silicate process of ester solidification, phosphate
Starch -130 parts of natural plant gum copolymerization adhesive, 80 parts of fiber, 5 parts of ammonium persulfate, 5 parts of polyvinyl alcohol, 20 parts of sodium carbonate, hydrogen peroxide
500 parts, 50 parts of dimethyl silicone rubber, 2 parts of absolute ethyl alcohol, 15 parts of silica particles, 20% 20 parts of aqueous sodium carbonate, hydroxide
20 parts of calcium, 2600 parts of water, 5 parts of triphenyl phosphorus, 27 parts of chloride hydrate rhodium, 16 parts of catalyst, 220 parts of natural plant gum.
Adhesive and water mixed solution are mainly prepared from by following steps：
20% aqueous sodium carbonate is added in phosphate ester starch-natural plant gum copolymerization adhesive, is then stirring and/or is surpassing
It is slowly added to react 0.1~12 hour at a temperature of ammonium persulfate and hydrogen peroxide, 0~80 DEG C under sound effect, after reaction terminates, adds
System pH is adjusted to 7 by sodium carbonate；
Fiber and silica particles are wrapped up with cloth, are put into above-mentioned steps, is distilled, 12-14 minutes, cloth bag is taken out, will
Fiber and white carbon mixing, dry, particle are made；
Take particle to be mixed with calcium hydroxide, add in the round-bottomed flask equipped with reflux condensing tube, add anhydrous after degassing
Ethanol, heating water bath to 90 DEG C of backflows is completely dissolved triphenyl phosphorus, then the hydration chlorine for being dissolved in ethanol is added from condenser pipe upper end
Change rhodium, reaction precipitate is filtered, washed, dried to permanent quality, obtaining catalyst three by nitrogen protection, return stirring reaction 2h
Phenylphosphine radium chloride RhCl (PPh3) 3；
Dimethyl silicone rubber is added in autoclave, catalyst RhCl (PPh3) 3 is added after deaeration, it is warming up to
100 DEG C, be passed through hydrogen to 5.6MPa, reaction discharges after 11 hours, and reaction product inserts 40 DEG C of vacuum after being condensed with isopropanol
72h is dried in baking oven；
It is added to after drying in natural plant gum, stirs, be added to the water.
General principle, principal character and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (5)
1. a kind of method for preparing industrial metasilicate adhesive, it is characterised in that：Comprise the following steps and be prepared from：
1) solid sodium hydroxide and silicon powder are compared into 2.5-3 according to weight:1 ratio is added in electric smelter, heating curve according to
8-10 DEG C/min is warming up to 200 DEG C, is then warming up to 320-350 DEG C according to 4-6 DEG C/min, and the solid is made after heating
Sodium hydroxide is melted, and is further continued for being warming up to 400-450 DEG C according to 4-6 DEG C/min, is stopped heating, until silicon powder reaction
Completely, sodium orthosilicate crude product is produced；
2) environment temperature where sodium orthosilicate crude product is increased to 100 DEG C~140 DEG C, is incubated 0.5~1 hour；Temperature is increased to
190 DEG C~210 DEG C, it is incubated 1~2 hour；Temperature is increased to 295 DEG C~305 DEG C, is incubated 1.8~2.5 hours；Again by the original
Sodium metasilicate crude product is cooled to less than 40 DEG C, makes the sodium orthosilicate crude product completion of cure, produces sodium silicate solid；
3) sodium silicate solid is dissolved in water, then filtered, obtain sodium silicate solution, added in the sodium silicate solution sub-
Niter cake generates precipitated silica and sodium sulfite solution, and the mixture of generation is filtered；
4) by a part for the filtrate produced at the end of step (3) and the sulfur dioxide haptoreaction, and the sulfurous acid of generation
Hydrogen sodium product is recycled to recycling in step (3)；
5) filter cake obtained at the end of step (3) is acidified, be filtered, washed and dried, obtain light silicon dioxide；
6) another part filtrate of the filtrate produced at the end of step (3) is concentrated and dried, obtains high-quality industrial metasilicate；
7) the high-quality industrial metasilicate of preparation is mixed with 2 times of resin emulsion, special adhesive and water is put into after mixing
In mixed solution, during, the water-gas produced using gas generator passes sequentially through cyclone dust collectors, exchanger and accumulation of heat
Room, regenerator is provided with interlayer, and the waste heat pipe connection of interlayer and gas generator is molten to mixing by the waste heat of gas generator
Liquid is incubated, and stirs homogeneous, stirring duration 3 minutes, stops insulation, and natural cooling, precipitation removes moisture removal, sediment is done
After dry, add in silica sand, be sufficiently mixed and produce waterglass adhesive.
2. a kind of method for preparing industrial metasilicate adhesive according to claim 1, it is characterised in that：Described is viscous
Jelly and water mixed solution are prepared from including following components：10-13 parts of self-setting silicate process of ester solidification, phosphate ester starch-plant
101-130 parts of thing glue copolymerization adhesive, 65-80 parts of fiber, 2-5 parts of ammonium persulfate, 3-5 parts of polyvinyl alcohol, 1-20 parts of sodium carbonate,
450-500 parts of hydrogen peroxide, 45-50 parts of dimethyl silicone rubber, 1-2 parts of absolute ethyl alcohol, 10-15 parts of silica particles, 20% carbonic acid
15-20 parts of sodium water solution, calcium hydroxide:10-20 parts, 2300-2600 parts of water, 2-5 parts of triphenyl phosphorus, chloride hydrate rhodium 20-27
Part, 13-16 parts of catalyst, 200-220 parts of natural plant gum.
3. a kind of method for preparing industrial metasilicate adhesive according to claim 2, it is characterised in that：Described is viscous
Jelly and water mixed solution are prepared from including following components：10 parts of self-setting silicate process of ester solidification, phosphate ester starch-natural plant gum
101 parts of copolymerization adhesive, 65 parts of fiber, 2 parts of ammonium persulfate, 3 parts of polyvinyl alcohol, 1 part of sodium carbonate, hydrogen peroxide:450 parts, diformazan
Base silicon rubber：45 parts, 1 part of absolute ethyl alcohol, 10 parts of silica particles, 20% 15 parts of aqueous sodium carbonate, 10 parts of calcium hydroxide, water
2300 parts, 2 parts of triphenyl phosphorus, 20 parts of chloride hydrate rhodium, 13 parts of catalyst, 200 parts of natural plant gum.
4. a kind of method for preparing industrial metasilicate adhesive according to claim 2, it is characterised in that：Described is viscous
Jelly and water mixed solution are prepared from including following components：13 parts of self-setting silicate process of ester solidification, phosphate ester starch-natural plant gum
130 parts of copolymerization adhesive, 80 parts of fiber, 5 parts of ammonium persulfate, 5 parts of polyvinyl alcohol, 20 parts of sodium carbonate, 500 parts of hydrogen peroxide, diformazan
50 parts of base silicon rubber, 2 parts of absolute ethyl alcohol, 15 parts of silica particles, 20% 20 parts of aqueous sodium carbonate, 20 parts of calcium hydroxide, water
2600 parts, 5 parts of triphenyl phosphorus, 27 parts of chloride hydrate rhodium, 16 parts of catalyst, 220 parts of natural plant gum.
5. a kind of method for preparing industrial metasilicate adhesive according to claim 2, it is characterised in that：Described is viscous
Jelly and water mixed solution are mainly prepared from by following steps：
20% aqueous sodium carbonate is added in phosphate ester starch-natural plant gum copolymerization adhesive, then made in stirring and/or ultrasound
It is slowly added to react 0.1~12 hour at a temperature of ammonium persulfate and hydrogen peroxide, 0~80 DEG C under, after reaction terminates, adds carbonic acid
System pH is adjusted to 7 by sodium；
Fiber and silica particles are wrapped up with cloth, are put into above-mentioned steps, is distilled, 12-14 minutes, cloth bag is taken out, by fiber
With white carbon mixing, dry, particle is made；
Take particle to be mixed with calcium hydroxide, add in the round-bottomed flask equipped with reflux condensing tube, the absolute ethyl alcohol added after degassing,
Heating water bath to 90 DEG C of backflows are completely dissolved triphenyl phosphorus, then are added from condenser pipe upper end and be dissolved in the chloride hydrate rhodium of ethanol,
Nitrogen is protected, return stirring reaction 2h, and reaction precipitate is filtered, washed, is dried to permanent quality, catalyst triphenylphosphine is obtained
Radium chloride RhCl (PPh3) 3；
Dimethyl silicone rubber is added in autoclave, catalyst RhCl (PPh3) 3 is added after deaeration, it is warming up to 100
DEG C, be passed through hydrogen to 5.6MPa, reaction discharges after 11 hours, and reaction product inserts 40 DEG C of vacuum drying oven after being condensed with isopropanol
Middle dry 72h；
It is added to after drying in natural plant gum, stirs, be added to the water.
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| CN108307845A (en) * | 2018-01-30 | 2018-07-24 | 靳月华 | A kind of multiple beta pruning high-precision improved tool |
| CN109181573A (en) * | 2018-08-15 | 2019-01-11 | 芜湖横路新材料科技有限公司 | Six layers of bond for corrugated board of one kind and its preparation process |
| CN109650396A (en) * | 2019-01-28 | 2019-04-19 | 安徽科昂纳米科技有限公司 | A kind of preparation method of aerosil and aerosil obtained |
| CN114105598A (en) * | 2021-12-20 | 2022-03-01 | 深圳市源锋兴业科技有限公司 | Antibacterial silica gel product and production process thereof |
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Application publication date: 20170825 |