CN108949071A - A kind of preparation method of low viscous lower shrinkage impregnant - Google Patents
A kind of preparation method of low viscous lower shrinkage impregnant Download PDFInfo
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- CN108949071A CN108949071A CN201810758173.8A CN201810758173A CN108949071A CN 108949071 A CN108949071 A CN 108949071A CN 201810758173 A CN201810758173 A CN 201810758173A CN 108949071 A CN108949071 A CN 108949071A
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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
- C09J133/00—Adhesives based on 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- 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
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- C09K3/12—Materials for stopping leaks, e.g. in radiators, in tanks
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The present invention relates to impregnant preparation technical fields, and in particular to a kind of preparation method of low viscous lower shrinkage impregnant.The present invention is with acrylic acid, methacrylic acid is monomer, dodecyl sodium sulfate is added, the substances such as sodium bicarbonate obtain acrylate latex, rheology filler will be made by oneself, vermiculite power, acrylate latex is mixed to get infiltration liquid, poly-vinyl alcohol solution is reacted with n-butanal again, infiltration liquid is added, wood powder, reinforcing agent obtains low viscous lower shrinkage impregnant, vermiculite power in infiltration liquid, polyvinyl alcohol and the intermolecular intersolubility of n-butanal can be made to increase, improve reaction conversion ratio, lignin can generate biggish steric hindrance in infiltration liquid, be conducive to improve the dispersion performance of acrylate particles in infiltration liquid, reinforcing agent accelerates the volatilization of aqueous volatile matter in aqueous emulsion, in addition, settled density of the infiltration liquid in metal works bonding can be improved in lignin, reduce shrinkage when infiltration liquid rapid curing, it has a extensive future.
Description
Technical field
The present invention relates to impregnant preparation technical fields, and in particular to a kind of preparation method of low viscous lower shrinkage impregnant.
Background technique
Casting, weldment and metallic sintered products, the die casting of mechanical industry production, are changed into solid-state from the liquid metal of melting
During metallics, often there is volume contraction, while in this process, can also generate different degrees of loose, stomata,
Minute crack and the defects of being mingled with, and largely effect on its quality and use.Some defects are not easy to be found, to processing after by
Pressure testing just goes wrong, and causes the waste of working hour and raw material.Therefore, in mechanical processing process, need to converted products into
Row sealing and reinforcement.Method of impregnation be exactly for such purpose and generate a kind of technique.Infiltration is that sealing medium is (usually low
The impregnant of viscosity) by naturally osmotic (i.e. micropore self-priming), the methods of vacuumize and pressurize in infiltration into microporous (fine crack), will stitch
Gap filling is full, and the sealing medium solidification in gap is then reached sealing seam by the methods of nature (room temperature), cooling or heating
The effect of gap.
Impregnant is the liquid being formulated by inorganic or organic matter.It is to be suitable for casting, weldment and powder metallurgy
One kind of the metallic articles such as part, die casting effectively sealing reinforcing agent, is the effective ways for improving mechanical product quality, yield rate.
Mainly there are silicic acid sodium form impregnant, the agent of acrylic ester type organic impregnating and resin type impregnant three using extensive impregnant at present
Major class.Inorganic impregnant is a kind of impregnant used earliest, since its viscosity is high, wellability is poor, infiltration qualification rate is low, just
Gradually replaced acrylic ester type impregnant.Resin type impregnant due to viscosity is excessive, need to be added diluent into
Row dilution, in diluent containing there are many be more toxic with the higher compound of volatility, all to environmental protection and safety, infiltration yield rate
Bring detrimental effect, thus just gradually replaced acrylic ester type impregnant.
Acrylic ester type impregnant is a kind of impregnant for most having application prospect now., small toxicity lower with viscosity, no
Containing volatile matter, the characteristics such as energy consumption is lower, yield rate is high, the lesser hole of size can be suitble to.But due to acrylate monomer
Cure shrinkage is big, the shrinking percentage of many monomers 15% or more, cause the impregnant be easy to appear in the curing process slight crack and
Secondary contraction gap influences repairing effect, and the impregnant is relatively soft, and modulus is low, and intensity is low, and heat resistance is poor, and density is again low,
It is big with the difference of metal.In addition, since acrylic ester type impregnant is not completely soluble in water, often adhering to after part infiltration
In piece surface, in order to remove these impregnants, suitable emulsifier is often added, the impregnant for adhering to piece surface is easy to
It is rinsed with water clean.If piece surface remains impregnant, appearance is not only influenced, the processing performance of process after also influencing, seriously
Possibility block inside parts channel.
Therefore, research and develop a kind of low viscosity, good fluidity, nontoxicity and can be achieved at the same time improve workpiece's qualification rate with
And the high impregnant of service life is of great significance under the conditions of high temperature and humidity.
Summary of the invention
Present invention mainly solves the technical issues of, it is big for current acrylic ester type impregnant cure shrinkage, lead to this
Impregnant is easy to appear slight crack and secondary contraction gap in the curing process, influences repairing effect, and resin type impregnant is viscous
It spends larger, makes impregnation step time extended defect, provide a kind of preparation method of low viscous lower shrinkage impregnant.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of low viscous lower shrinkage impregnant, it is characterised in that specific preparation step are as follows:
(1) 200~230g stalk slag, 400~450mL sodium hydroxide solution are put into the water-bath kettle with blender,
Heating water bath heating DEG C, starts blender, stirs 3~5h, obtains lignin lye, and lignin lye glacial acetic acid is adjusted pH
It is moved into supercentrifuge after to neutrality, 12~15min of high speed centrifugation, removes supernatant liquor, isolated lower sediment uses water
It is moved into baking oven after washing precipitating 2~3 times, is dried to obtain wood powder, it is spare；
(2) 70~75g beta-cyclodextrin and 100~130mL sodium hydroxide solution are added into beaker, stir 10 at room temperature~
After 15min, 5~10g2 is added, 3- epoxypropyltrimethylchloride chloride places the beaker in water-bath, heat temperature raising, heat preservation
Reaction, filtering removal filtrate obtains reinforcing agent, spare；
(3) according to parts by weight, 20~30 parts of epoxidized soybean oils, 50~60 parts of distilled water, 10~15 are added into three-necked flask
Part dodecyl sodium sulfate, 4~5 parts of sodium bicarbonates, 40~45 parts of acrylic acid and 20~30 parts of methacrylic acids, then leaked with dropping liquid
It struggles against and 1~3 part of potassium peroxydisulfate is added dropwise into four-hole boiling flask, after being added dropwise, insulation reaction continues heat temperature raising, insulation reaction, drop
Temperature adjusts pH with ammonium hydroxide, and discharging obtains acrylate latex；
(4) according to parts by weight, take 60~70 parts of EVA resins, 20~25 parts of phenyl silicone oils, 10~15 parts of fumed silicas mixed
It closes, obtains rheology filler, take vermiculite to be put into ball milling in ball mill, sieving obtains vermiculite power, by vermiculite power, rheology filler, propylene
The mixing of acid esters latex, obtains infiltration liquid；
(5) according to parts by weight, 40~50 parts of poly-vinyl alcohol solutions are squeezed into condensation reaction kettle through filter and is cooled down, dropped
30~40 parts of n-butanals, 3~4 parts of benzene sulfonic acids are sequentially added after temperature, and 40~50 parts of infiltrations are added after reaction into condensation reaction kettle
Liquid, the reaction was continued is mutually layered until reacting in condensation reaction kettle, is mutually layered subsequent temperature of continuing rising to react in condensation reaction kettle, instead
It answers, is separated by filtration removal upper layer waste liquid, continue that 70~80 parts of infiltration liquids, 10~12 parts of wood powders are added into condensation reaction kettle,
20~25 reinforcing agents, heating, insulated and stirred processing obtain low viscous lower shrinkage impregnant.
The mass fraction of sodium hydroxide solution described in step (1) is 45%, and heating water bath heating is 90~95 DEG C, ice vinegar
Acid mass fraction is 95%, and high speed centrifugation revolving speed is 3500~3700r/min, and baking oven set temperature is 70~80 DEG C, drying time
For 4~5h.
The mass fraction of sodium hydroxide solution described in step (2) is 90%, and heat temperature raising is 50~55 DEG C, insulation reaction
Time is 3~4h.
Dropping funel drop rate described in step (3) is 3~5mL/min, and the insulation reaction time is 30~40min, is added
Heat heating is 90~100 DEG C, and the insulation reaction time is 45~55min, and reducing temperature is 55~60 DEG C, and the mass fraction of ammonium hydroxide is
20%, it is 6.0~7.0 that ammonium hydroxide, which adjusts pH,.
Vinyl acetate mass content is 25~30% in EVA resin described in step (4), and Ball-milling Time is 30~40min,
Be sieved specification is 400 mesh, and vermiculite power, rheology filler, acrylate latex mixing mass ratio are 1 ︰, 3 ︰ 7.
The mass fraction of poly-vinyl alcohol solution described in step (5) is 40%, and temperature is 10~15 DEG C, when reaction after cooling
Between be 40~50min, continue heating as 55~60 DEG C, the reaction time is 10~15h after heating, and temperature is 70~78 after heating
DEG C, insulated and stirred handles the time as 45~50min.
The beneficial effects of the present invention are:
(1) objects such as distilled water, dodecyl sodium sulfate, sodium bicarbonate are added using acrylic acid, methacrylic acid as monomer in the present invention
Matter continues to add epoxidized soybean oil, initiator after heating stirring is reacted, and adjusts pH again by cross-linking reaction with ammonium hydroxide, obtains
To acrylate latex, ethylene-vinyl acetate copolymer, phenyl silicone oil, fumed silica are mixed to get rheology filler,
Rheology filler, vermiculite power, acrylate latex are mixed to get infiltration liquid by certain mass ratio, by poly-vinyl alcohol solution and positive fourth
Aldehyde, which is placed in condensation reaction kettle, to react, removal upper layer waste liquid after layering, addition infiltration liquid, wood powder, reinforcing agent, at insulated and stirred
Reason, obtains low viscous lower shrinkage impregnant, the present invention intersects polycondensation by using polyvinyl alcohol and n-butanal, utilizes acidic catalyst
Benzene sulfonic acid, prepares the polyvinyl butyral that can be dissolved each other with acrylate, and the vermiculite power in infiltration liquid can make polyethylene
Alcohol and the intermolecular intersolubility of n-butanal increase, and improve reaction conversion ratio, since the viscosity of polyvinyl butyral is lower, and
The porous structure of vermiculite power can inhibit polyvinyl butyral to crystallize the curing time for being hardened and extending acrylate, so that infiltration
Agent viscosity reduces, and has preferable mobility；
(2) modified material of the wood powder that is recycled using in stalk slag as infiltration liquid, lignin itself in wood powder in the present invention
With biggish space structure, biggish steric hindrance can be generated in infiltration liquid, be conducive to improve acrylate in infiltration liquid
The dispersion performance of particle makes each region of infiltration liquid keep uniform density, reduces the shrinkage for solidifying the later period, by pasting β-ring
Essence 2,3- epoxypropyltrimethylchloride chloride carries out cationic etherificate, reinforcing agent is prepared, the reinforcing agent is in aqueous emulsion
Can and the acrylate for the electronics that is easy to get between generate electrostatic attraction effect, the electrostatic attraction act on so that polymeric groups in and point
Association can be generated in subchain, polymer molecule is caused to shrink, and hydrodynamic volume reduces, and accelerates waving for aqueous volatile matter
Hair improves infiltration liquid when metal works bond in addition, phase lignin can increase the average molecular weight of infiltration liquid after hardening
Settled density reduces shrinkage when infiltration liquid rapid curing, has a extensive future.
Specific embodiment
200~230g stalk slag, the sodium hydroxide solution that 400~450mL mass fraction is 45% are put into blender
Water-bath kettle in, heating water bath is warming up to 90~95 DEG C, starts blender, stirs 3~5h, obtains lignin lye, will
The glacial acetic acid that lignin lye mass fraction is 95% moves into supercentrifuge after adjusting pH to neutrality, with 3500~
The revolving speed of 3700r/min, 12~15min of high speed centrifugation remove supernatant liquor, and precipitating 2 is washed with water in isolated lower sediment
It is moved into after~3 times in the baking oven that set temperature is 70~80 DEG C, dry 4~5h obtains wood powder, spare；It is added into beaker
The sodium hydroxide solution that 70~75g beta-cyclodextrin and 100~130mL mass fraction are 90%, after stirring 10~15min at room temperature,
5~10g2 is added, 3- epoxypropyltrimethylchloride chloride places the beaker in water-bath, is heated to 50~55 DEG C, protects
Temperature 3~4h of reaction, filtering removal filtrate obtains reinforcing agent, spare；According to parts by weight, 20~30 parts are added into three-necked flask
Epoxidized soybean oil, 50~60 parts of distilled water, 10~15 parts of dodecyl sodium sulfates, 4~5 parts of sodium bicarbonates, 40~45 parts of propylene
Acid and 20~30 parts of methacrylic acids, then 1~3 is added dropwise with the drop rate of 3~5mL/min into four-hole boiling flask with dropping funel
Part potassium peroxydisulfate, after being added dropwise, 30~40min of insulation reaction continues to be heated to 90~100 DEG C, and insulation reaction 45~
55min is cooled to 55~60 DEG C, and it is 6.0~7.0 that the ammonium hydroxide for being 20% with mass fraction, which adjusts pH, and discharging obtains acrylate
Latex；According to parts by weight, take 60~70 parts of EVA resins, 20~25 parts of phenyl silicone oils, 10~15 parts of fumed silicas mixed
It closes, obtains rheology filler, wherein vinyl acetate mass content is 25~30% in EVA resin, and vermiculite is taken to be put into ball milling in ball mill
30~40min crosses 400 meshes and obtains vermiculite power, is in mass ratio that 1 ︰, 3 ︰ 7 is mixed by vermiculite power, rheology filler, acrylate latex
It closes, obtains infiltration liquid；According to parts by weight, the poly-vinyl alcohol solution that 40~50 parts of mass fractions are 40% is squeezed into through filter
Cool down in condensation reaction kettle, 30~40 parts of n-butanals, 3~4 parts of benzene sulfonic acids are sequentially added after being cooled to 10~15 DEG C, reacts
40~50 parts of infiltration liquids are added after 40~50min into condensation reaction kettle, the reaction was continued until reaction phase is divided in condensation reaction kettle
Layer is continuously heating to 55~60 DEG C after reacting mutually layering in condensation reaction kettle, reacts 10~15h, is separated by filtration removal upper layer
Waste liquid continues that 70~80 parts of infiltration liquids, 10~12 parts of wood powders are added into condensation reaction kettle, and 20~25 reinforcing agents are warming up to
70~78 DEG C, insulated and stirred handles 45~50min, obtains low viscous lower shrinkage impregnant.
200g stalk slag, the sodium hydroxide solution that 400mL mass fraction is 45% are put into the water-bath with blender
In kettle, heating water bath is warming up to 90 DEG C, starts blender, stirs 3h, obtains lignin lye, by lignin lye quality point
Number moves into supercentrifuge after adjusting pH to neutrality for 95% glacial acetic acid, with the revolving speed of 3500r/min, high speed centrifugation
12min, removes supernatant liquor, and isolated lower sediment moves into the baking oven that set temperature is 70 DEG C after being washed with water precipitating 2 times
In, dry 4h obtains wood powder, spare；The hydroxide that 70g beta-cyclodextrin and 100mL mass fraction are 90% is added into beaker
Sodium solution adds 5g2 after stirring 10min at room temperature, and 3- epoxypropyltrimethylchloride chloride places the beaker in water-bath,
50 DEG C, insulation reaction 3h are heated to, filtering removal filtrate obtains reinforcing agent, spare；According to parts by weight, to three-necked flask
20 parts of epoxidized soybean oils of middle addition, 50 parts of distilled water, 10 parts of dodecyl sodium sulfates, 4 parts of sodium bicarbonates, 40 parts of acrylic acid and 20
Part methacrylic acid, then 1 part of potassium peroxydisulfate is added dropwise with the drop rate of 3mL/min into four-hole boiling flask with dropping funel, it is added dropwise
After, insulation reaction 30min continues to be heated to 90 DEG C, insulation reaction 45min, is cooled to 55 DEG C, is with mass fraction
It is 6.0 that 20% ammonium hydroxide, which adjusts pH, and discharging obtains acrylate latex；According to parts by weight, 60 parts of EVA resins, 20 parts of benzene are taken
Base silicone oil, 10 parts of fumed silica mixing, obtain rheology filler, and wherein vinyl acetate mass content is 25% in EVA resin,
It takes vermiculite to be put into ball milling 30min in ball mill, crosses 400 meshes and obtain vermiculite power, by vermiculite power, rheology filler, acrylic adhesive
Cream mixes in mass ratio for 1 ︰, 3 ︰ 7, obtains infiltration liquid；According to parts by weight, 40 parts of mass fractions are molten for 40% polyvinyl alcohol
Liquid is squeezed into condensation reaction kettle through filter to cool down, and 30 parts of n-butanals, 3 parts of benzene sulfonic acids are sequentially added after being cooled to 10 DEG C,
40 parts of infiltration liquids are added into condensation reaction kettle after reacting 40min, the reaction was continued is mutually layered until reacting in condensation reaction kettle, to
55 DEG C are continuously heating to after reacting mutually layering in condensation reaction kettle, reacts 10h, removal upper layer waste liquid is separated by filtration, continues to contracting
It closes and 70 parts of infiltration liquids, 10 parts of wood powders is added in reaction kettle, 20 reinforcing agents are warming up to 70 DEG C, and insulated and stirred handles 45min, obtains
To low viscous lower shrinkage impregnant.
215g stalk slag, the sodium hydroxide solution that 425mL mass fraction is 45% are put into the water-bath with blender
In kettle, heating water bath is warming up to 93 DEG C, starts blender, stirs 4h, obtains lignin lye, by lignin lye quality point
Number moves into supercentrifuge after adjusting pH to neutrality for 95% glacial acetic acid, with the revolving speed of 3600r/min, high speed centrifugation
13min, removes supernatant liquor, and isolated lower sediment moves into the baking oven that set temperature is 75 DEG C after being washed with water precipitating 2 times
In, dry 4h obtains wood powder, spare；The hydroxide that 73g beta-cyclodextrin and 115mL mass fraction are 90% is added into beaker
Sodium solution adds 7g2 after stirring 13min at room temperature, and 3- epoxypropyltrimethylchloride chloride places the beaker in water-bath,
53 DEG C, insulation reaction 3h are heated to, filtering removal filtrate obtains reinforcing agent, spare；According to parts by weight, to three-necked flask
25 parts of epoxidized soybean oils of middle addition, 55 parts of distilled water, 13 parts of dodecyl sodium sulfates, 4 parts of sodium bicarbonates, 43 parts of acrylic acid and 25
Part methacrylic acid, then 2 parts of potassium peroxydisulfates are added dropwise with the drop rate of 4mL/min into four-hole boiling flask with dropping funel, it is added dropwise
After, insulation reaction 35min continues to be heated to 95 DEG C, insulation reaction 50min, is cooled to 57 DEG C, is with mass fraction
It is 6.5 that 20% ammonium hydroxide, which adjusts pH, and discharging obtains acrylate latex；According to parts by weight, 65 parts of EVA resins, 23 parts of benzene are taken
Base silicone oil, 13 parts of fumed silica mixing, obtain rheology filler, and wherein vinyl acetate mass content is 27% in EVA resin,
It takes vermiculite to be put into ball milling 35min in ball mill, crosses 400 meshes and obtain vermiculite power, by vermiculite power, rheology filler, acrylic adhesive
Cream mixes in mass ratio for 1 ︰, 3 ︰ 7, obtains infiltration liquid；According to parts by weight, 45 parts of mass fractions are molten for 40% polyvinyl alcohol
Liquid is squeezed into condensation reaction kettle through filter to cool down, and 35 parts of n-butanals, 3 parts of benzene sulfonic acids are sequentially added after being cooled to 13 DEG C,
45 parts of infiltration liquids are added into condensation reaction kettle after reacting 45min, the reaction was continued is mutually layered until reacting in condensation reaction kettle, to
57 DEG C are continuously heating to after reacting mutually layering in condensation reaction kettle, reacts 13h, removal upper layer waste liquid is separated by filtration, continues to contracting
It closes and 75 parts of infiltration liquids, 11 parts of wood powders is added in reaction kettle, 23 reinforcing agents are warming up to 74 DEG C, and insulated and stirred handles 47min, obtains
To low viscous lower shrinkage impregnant.
230g stalk slag, the sodium hydroxide solution that 450mL mass fraction is 45% are put into the water-bath with blender
In kettle, heating water bath is warming up to 95 DEG C, starts blender, stirs 5h, obtains lignin lye, by lignin lye quality point
Number moves into supercentrifuge after adjusting pH to neutrality for 95% glacial acetic acid, with the revolving speed of 3700r/min, high speed centrifugation
15min, removes supernatant liquor, and isolated lower sediment moves into the baking oven that set temperature is 80 DEG C after being washed with water precipitating 3 times
In, dry 5h obtains wood powder, spare；The hydroxide that 75g beta-cyclodextrin and 130mL mass fraction are 90% is added into beaker
Sodium solution adds 10g2,3- epoxypropyltrimethylchloride chloride places the beaker water-bath after stirring 15min at room temperature
In, 55 DEG C, insulation reaction 4h are heated to, filtering removal filtrate obtains reinforcing agent, spare；According to parts by weight, Xiang Sankou
30 parts of epoxidized soybean oils, 60 parts of distilled water, 15 parts of dodecyl sodium sulfates, 5 parts of sodium bicarbonates, 45 parts of acrylic acid are added in flask
With 30 parts of methacrylic acids, then with dropping funel 3 parts of potassium peroxydisulfates are added dropwise with the drop rate of 5mL/min into four-hole boiling flask,
After being added dropwise, insulation reaction 40min continues to be heated to 100 DEG C, and insulation reaction 55min is cooled to 60 DEG C, uses quality
It is 7.0 that the ammonium hydroxide that score is 20%, which adjusts pH, and discharging obtains acrylate latex；According to parts by weight, take 70 parts of EVA resins,
25 parts of phenyl silicone oils, 15 parts of fumed silica mixing, obtain rheology filler, wherein vinyl acetate mass content in EVA resin
It is 30%, vermiculite is taken to be put into ball milling 40min in ball mill, crosses 400 meshes and obtain vermiculite power, by vermiculite power, rheology filler, propylene
Acid esters latex is 1 ︰, 3 ︰ 7 mixing in mass ratio, obtains infiltration liquid；According to parts by weight, the poly- second for being 40% by 50 parts of mass fractions
Enolate solution is squeezed into condensation reaction kettle through filter to cool down, and 40 parts of n-butanals, 4 parts of benzene are sequentially added after being cooled to 15 DEG C
50 parts of infiltration liquids are added into condensation reaction kettle after reacting 50min for sulfonic acid, and the reaction was continued until reaction phase is divided in condensation reaction kettle
Layer is continuously heating to 60 DEG C after reacting mutually layering in condensation reaction kettle, reacts 15h, is separated by filtration removal upper layer waste liquid, continues
80 parts of infiltration liquids, 12 parts of wood powders are added into condensation reaction kettle, 25 reinforcing agents are warming up to 78 DEG C, insulated and stirred processing
50min obtains low viscous lower shrinkage impregnant.
The impregnant that comparative example is produced with Nanjing company as a comparison case soaks low viscous lower shrinkage produced by the present invention
Impregnant in penetration enhancer and comparative example is detected, and testing result is as shown in table 1:
Density measurement is tested by " GB/T13354 liquid adhesive density measurement method-weight agar diffusion method ".
Viscosimetric analysis is tested by " the measurement list cylinder rotary viscosimeter method of GB/T2794-2013 adhesive viscosity ".
The measurement of solidfied material water absorption rate exists the impregnant in low viscous lower shrinkage impregnant produced by the present invention and comparative example
Casting film-forming on silica gel plate, is then placed in baking oven, solidifies at 90 DEG C, prepares the glue film that thickness is about 1mm.Glue film is cut
It at the fritter of 3cm × 3cm, weighs (quality W0), is put into after impregnating 48h in tap water and takes out, blot surface moisture with filter paper,
It weighs (quality W1), by formula: water absorption rate=(W1-W0)/W0 × 100% calculates water absorption rate.
1 performance measurement result of table
| Test item | Example 1 | Example 2 | Example 3 | Comparative example |
| Density (g/cm3) | 1.062 | 1.061 | 1.059 | 1.148 |
| Appearance | Colourless transparent oil liquid | Colourless transparent oil liquid | Colourless transparent oil liquid | Colourless transparent oil liquid |
| Viscosity (mPas) | 9.56 | 9.52 | 9.47 | 16.32 |
| Curing time (s) | 165 | 162 | 157 | 244 |
| Cubical contraction (%) | 2.0 | 1.8 | 1.7 | 15.7 |
| Washing property | Without residue glue | Without residue glue | Without residue glue | There is a small amount of residue glue |
| Stability (75 DEG C × 20min) | Not gel | Not gel | Not gel | Not gel |
| Solidfied material water absorption rate (%) | 0.51 | 0.47 | 0.47 | 0.97 |
| Solidfied material hardness (D) | 97.9 | 98.6 | 99.2 | 86.1 |
According to data in table 1 it is found that low viscous lower shrinkage impregnant viscosity produced by the present invention is low, good fluidity, nontoxicity, be free of
Volatile matter is particularly suitable for using in mechanical industry field, and simple process, and raw material sources are extensive, before having wide use
Scape.
Claims (6)
1. a kind of preparation method of low viscous lower shrinkage impregnant, it is characterised in that specific preparation step are as follows:
(1) 200~230g stalk slag, 400~450mL sodium hydroxide solution are put into the water-bath kettle with blender,
Heating water bath heating DEG C, starts blender, stirs 3~5h, obtains lignin lye, and lignin lye glacial acetic acid is adjusted pH
It is moved into supercentrifuge after to neutrality, 12~15min of high speed centrifugation, removes supernatant liquor, isolated lower sediment uses water
It is moved into baking oven after washing precipitating 2~3 times, is dried to obtain wood powder, it is spare；
(2) 70~75g beta-cyclodextrin and 100~130mL sodium hydroxide solution are added into beaker, stir 10 at room temperature~
After 15min, 5~10g2 is added, 3- epoxypropyltrimethylchloride chloride places the beaker in water-bath, heat temperature raising, heat preservation
Reaction, filtering removal filtrate obtains reinforcing agent, spare；
(3) according to parts by weight, 20~30 parts of epoxidized soybean oils, 50~60 parts of distilled water, 10~15 are added into three-necked flask
Part dodecyl sodium sulfate, 4~5 parts of sodium bicarbonates, 40~45 parts of acrylic acid and 20~30 parts of methacrylic acids, then leaked with dropping liquid
It struggles against and 1~3 part of potassium peroxydisulfate is added dropwise into four-hole boiling flask, after being added dropwise, insulation reaction continues heat temperature raising, insulation reaction, drop
Temperature adjusts pH with ammonium hydroxide, and discharging obtains acrylate latex；
(4) according to parts by weight, take 60~70 parts of EVA resins, 20~25 parts of phenyl silicone oils, 10~15 parts of fumed silicas mixed
It closes, obtains rheology filler, take vermiculite to be put into ball milling in ball mill, sieving obtains vermiculite power, by vermiculite power, rheology filler, propylene
The mixing of acid esters latex, obtains infiltration liquid；
(5) according to parts by weight, 40~50 parts of poly-vinyl alcohol solutions are squeezed into condensation reaction kettle through filter and is cooled down, dropped
30~40 parts of n-butanals, 3~4 parts of benzene sulfonic acids are sequentially added after temperature, and 40~50 parts of infiltrations are added after reaction into condensation reaction kettle
Liquid, the reaction was continued is mutually layered until reacting in condensation reaction kettle, is mutually layered subsequent temperature of continuing rising to react in condensation reaction kettle, instead
It answers, is separated by filtration removal upper layer waste liquid, continue that 70~80 parts of infiltration liquids, 10~12 parts of wood powders are added into condensation reaction kettle,
20~25 reinforcing agents, heating, insulated and stirred processing obtain low viscous lower shrinkage impregnant.
2. the preparation method of the low viscous lower shrinkage impregnant of one kind according to claim 1, it is characterised in that: step (1) institute
The mass fraction for the sodium hydroxide solution stated is 45%, and heating water bath heating is 90~95 DEG C, and glacial acetic acid mass fraction is 95%, high
Fast centrifugal rotational speed is 3500~3700r/min, and baking oven set temperature is 70~80 DEG C, and drying time is 4~5h.
3. the preparation method of the low viscous lower shrinkage impregnant of one kind according to claim 1, it is characterised in that: step (2) institute
The mass fraction for the sodium hydroxide solution stated is 90%, and heat temperature raising is 50~55 DEG C, and the insulation reaction time is 3~4h.
4. the preparation method of the low viscous lower shrinkage impregnant of one kind according to claim 1, it is characterised in that: step (3) institute
The dropping funel drop rate stated is 3~5mL/min, and the insulation reaction time is 30~40min, and heat temperature raising is 90~100 DEG C,
The insulation reaction time is 45~55min, and reducing temperature is 55~60 DEG C, and the mass fraction of ammonium hydroxide is 20%, and ammonium hydroxide adjusts pH and is
6.0~7.0.
5. the preparation method of the low viscous lower shrinkage impregnant of one kind according to claim 1, it is characterised in that: step (4) institute
Vinyl acetate mass content is 25~30% in the EVA resin stated, and Ball-milling Time is 30~40min, and be sieved specification is 400 mesh,
Vermiculite power, rheology filler, acrylate latex mixing mass ratio are 1 ︰, 3 ︰ 7.
6. the preparation method of the low viscous lower shrinkage impregnant of one kind according to claim 1, it is characterised in that: step (5) institute
The mass fraction for the poly-vinyl alcohol solution stated is 40%, and temperature is 10~15 DEG C after cooling, and the reaction time is 40~50min, is continued
Heating is 55~60 DEG C, and the reaction time is 10~15h after heating, and temperature is 70~78 DEG C after heating, and insulated and stirred handles the time
For 45~50min.
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