CN105670535A - Preparation method and application method of formaldehyde-free and environment-friendly type water-tolerant and high-strength adhesives - Google Patents
Preparation method and application method of formaldehyde-free and environment-friendly type water-tolerant and high-strength adhesives Download PDFInfo
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- CN105670535A CN105670535A CN201610259037.5A CN201610259037A CN105670535A CN 105670535 A CN105670535 A CN 105670535A CN 201610259037 A CN201610259037 A CN 201610259037A CN 105670535 A CN105670535 A CN 105670535A
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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
- C09J125/00—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 an aromatic carbocyclic ring; Adhesives based on derivatives of such polymers
- C09J125/02—Homopolymers or copolymers of hydrocarbons
- C09J125/04—Homopolymers or copolymers of styrene
- C09J125/08—Copolymers of styrene
- C09J125/14—Copolymers of styrene with unsaturated esters
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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
- C08F212/00—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 aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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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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- Inorganic Chemistry (AREA)
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- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a preparation method and an application method of formaldehyde-free and environment-friendly type water-tolerant and high-strength adhesives, and belongs to the field of adhesives. The preparation method of the adhesives sequentially comprises a waterproof emulsion preparation method and an adhesive compounding method. The adhesives prepared with the preparation method are formaldehyde-free, green and environment-friendly, have high adhesion strength and good water tolerance, can be widely applied to fields closely related to human life, such as home decoration, artificial boards and the like, are basically harmless to the environment and human bodies, and are widely applied to plate pressing and laminating with wood, and suitable for hard wood and soft wood of various specifications.
Description
Technical field
The invention belongs to adhesive field, be specifically related to preparation and the using method thereof of the water-fast high-strength adhesive of a kind of timber aldehyde-free environment-friendly.
Background technology
Along with the raising of socioeconomic development and living standards of the people, to the demand of wood materials also in continuous increase, the traditional diamond-making technique of wood materials can not meet the demand of socio-economic development. Since reform and opening-up, China's adhesive industry development is rapid, yield sharp increase, quality improves constantly, and application expands to the industries such as building industry, paper products and packaging, shoemaking, automobile, electronics, carpenter, household electrical appliance, house equipment, transport, space flight and aviation and health care gradually. It is reported, China adhesive produces and disperses very much, has extensive and high-caliber producer only various schools of thinkers, most enterprises production technology level is low, equipment outmoded simple and crude, science and technology strength is weak, product quality is not high, three waste discharge does not meet national requirements for environmental protection. Some indexs of correlation lack corresponding examination requirements and standard, and this series of problems makes adhesive industry there is the bigger wasting of resources and problem of environmental pollution. The most effective method solving this contradiction is to utilize adhesive bonding technique, is undertaken glueing joint, recombinating and Compound Machining by different size, lignocellulose raw material of different nature, produces and is applicable to the different sheet material of instructions for use, square bar and pressing etc. These all be unable to do without adhesive and adhesive bonding technique. For this, adhesive and the adhesive bonding technique status in wood processing field just seems even more important. Showing according to China's Industry Information Network data, within 2012, annual wood-based plate yield is 28568 ten thousand steres, increases by 19.72% than the same period in 2010. Owing to the demand of wood-based plate and yield are increased sharply, increasing also very fast to adhesive demand required in production process, the wood-based plate such as plywood, particieboard, furniture, fibre board uses the based Wood Adhesives accounting for 90%, accounts for the largest percentage. China there are about the adhesive of 70% for wood-processing industry.
" three-aldehyde glue " that current wood processing field commonly uses: the i.e. glutinous agent of Lauxite, phenolic resin and melamine-formaldehyde resin adhesive. But three-aldehyde glue discharges substantial amounts of formaldehyde in the process produced and use, especially in indoor decoration and Furniture panel, because formaldehyde not exclusively polycondensation, considerable part is often had to exist with free state, can disperse towards periphery gradually and cause environmental pollution, causing contaminated environment and harm public health, the negative effect that environment and human lives's aspect are in use caused by three-aldehyde glue has caused the extensive attention of countries in the world.In recent years, along with the enhancing that appearance and the health of people of environmental regulation are realized, country is more and more stricter to the volatilization quantitative limitation of acetals adhesive Free-formaldehyde. Timber industry adhesive industry is faced with inevitable challenge. Therefore, exploitation non-toxic, environmental friendly based Wood Adhesives will be research emphasis from now on.
For this reason, it is necessary to research and develop a kind of timber Aqueous Adhesives by the water-fast high intensity of height nontoxic, environmental type, i.e. the preparation of the water-fast high-strength adhesive of a kind of timber aldehyde-free environment-friendly and using method thereof.
Summary of the invention
It is an object of the invention to provide the preparation of the water-fast high-strength adhesive of a kind of timber aldehyde-free environment-friendly and using method thereof, prepared adhesive is without formaldehyde, environmental protection, adhesive strength height, resistance to water is better, can at house decoration and artificial board etc. closely and extensive use in human lives's association area, environment and human body is substantially harmless, it is widely used in first timber pressing plate, the use of jigsaw, is suitable for hardwood, the multiple timber and lumber standards of cork.
For achieving the above object, the present invention adopts the following technical scheme that
The preparation method of a kind of timber aldehyde-free environment-friendly is water-fast high-strength adhesive, the preparation method of described adhesive includes the preparation method of water-proof emulsion and the preparation method of adhesive successively.
Preferably, the preparation method of described water-proof emulsion specifically includes following steps:
A1. in pre-emulsification still one, first adding the deionized water of 8 weight portions, add the N n-methylolacrylamide of 1 weight portion and the N-[2-(2-methyl-4-oxopentyl) of 0.28 weight portion, stirring 15min, until being completely dissolved;
A2. the solution after dissolving to described step A1 adds emulsifying agent, stirs 15min, slowly take out the monomer butyl acrylate adding 10 weight portions, abundant pre-emulsification;
A3. in pre-emulsified product abundant in step A2, it is initially charged the butyl acrylate of 13 weight portions, sequentially adds the acrylic acid of the styrene of 19 weight portions, the methymethacrylate of 2.8 weight portions and 1.1 weight portions, obtain pre-emulsion;
A4. in pre-emulsification still two, add the deionized water of 5 weight portions, add emulsifying agent, be then sequentially added into the acrylic acid of the styrene of 2.8 weight portions, the methymethacrylate of 2.2 weight portions and 1.1 weight portions, after fully emulsified emulsified monomer;
A5. the water of 34 weight portions is added to reactor one, when low whipping speed is warming up to 72 DEG C when being 30r/min, add the sodium bicarbonate of 0.06 weight portion, continue to add when stirring is warming up to 82 DEG C the initiator ammonium persulfate of 0.06 weight portion, 30min is until being completely dissolved in reaction, continuing stirring to heat up until when temperature goes up to 84 DEG C, starting to drip the pre-emulsion of the step A3 gained of 0.6 weight portion, time for adding is 2.5～3 hours;
A6. after described step A5 dropwises, continuing to drip the emulsified monomer of step A4 gained in described reactor one, time for adding is 1～1.5 hour, after dropwising, is incubated 30 minutes under 84 DEG C of conditions,
A7. in described step A6 products therefrom, add the initiator ammonium persulfate of 0.002 weight portion and the deionized water of 0.1 weight portion, be warming up to 90 DEG C and be incubated 1 hour,
A8. it is incubated after 1h reaction until described step A7 and is cooled to 65～70 DEG C immediately, drip the tert-butyl hydroperoxide of 0.001 weight portion, time for adding is 10 minutes, when being then cooled to 56～60 DEG C, drip the sodium formaldehyde sulfoxylate of 0.0015 weight portion, time for adding is 30 minutes, is cooled to 50 DEG C after dropwising, and namely prepares water-proof emulsion.
Preferably, the preparation method of described adhesive specifically includes following steps:
B1. first add the water-proof emulsion of step A8 gained to reactor two, add 800 order dicalcium powders, be sufficiently stirred for 1 hour;
B2., after described step B1 stirs, add polyvinyl alcohol aqueous emulsion, stir 1 hour;
B3. after described step B2 stirs, add deionized water, stir 30min discharging, obtain adhesive to be prepared.
Preferably, polyvinyl alcohol aqueous emulsion described in step B2 to be model be 2488 polyvinyl alcohol be dissolved as the aqueous emulsion that mass fraction is 17%～19%.
Preferably, the volume ratio of described water-proof emulsion, dicalcium powder, polyvinyl alcohol aqueous emulsion and deionized water is 3～4:3～4:3:1～2.
Preferably, the using method of a kind of timber aldehyde-free environment-friendly is water-fast high-strength adhesive, comprise the steps:
C1. before using, described adhesive and firming agent are compared according to the quality of 1:10 and mix homogeneously;
C2. adopt artificial or machine roller coating method that the product after described step C1 gained mix homogeneously is coated on wood surface, and desirable gluing effect within 40 minutes, can be obtained 50 tons of pressure conjunctions.
Preferably, in described step C1, firming agent is isocyanates.
The beneficial effects of the present invention is,
(1) adhesive environmental protection prepared by the present invention, adhesive strength are high, and resistance to water is better;
(2) adhesive prepared by the present invention is without formaldehyde, can at house decoration and artificial board etc. closely and extensive use in human lives's association area, environment and human body is substantially harmless, Environmental Safety;
(3) adhesive prepared by the present invention and isocyanate curing agent fit in Bi-component adhesive, product has interior soft outer soft, structural strength high feature, with firming agent with the use of reaching D4 water protection standards, it is widely used in first timber pressing plate, the use of jigsaw, is suitable for hardwood, the multiple timber and lumber standards of cork;
(4) the preparation method technique of adhesive provided by the invention is simple, without " three wastes " discharge, with low cost.
Detailed description of the invention
For the technological means making the present invention realize, creation characteristic, reach purpose and effect and be easy to understand, below in conjunction with detailed description of the invention, the present invention is expanded on further.
Embodiment
The preparation method of a kind of timber aldehyde-free environment-friendly is water-fast high-strength adhesive, includes the preparation method of water-proof emulsion and the preparation method of adhesive successively.
The preparation method of described water-proof emulsion specifically includes as follows:
A1. in pre-emulsification still one, first add 8g deionized water, adding 1gN n-methylolacrylamide and 0.28g N-[2-(2-methyl-4-oxopentyl), stirring 15min, until being completely dissolved;
A2. the solution after dissolving to described step A1 adds emulsifying agent, stirs 15min, slowly take out and add 10g monomer butyl acrylate, abundant pre-emulsification;
A3. in pre-emulsified product abundant in step A2, it is initially charged 13g butyl acrylate, sequentially adds 19g styrene, 2.8g methymethacrylate and 1.1g acrylic acid, obtain pre-emulsion;
A4. in pre-emulsification still two, add 5g deionized water, add emulsifying agent, be then sequentially added into 2.8g styrene, 2.2g methymethacrylate and 1.1g acrylic acid, after fully emulsified, obtain emulsified monomer;
A5. 34g water is added to reactor one, when low whipping speed is warming up to 72 DEG C when being 30r/min, add 0.06g sodium bicarbonate, continue to add 0.06g initiator ammonium persulfate when stirring is warming up to 82 DEG C, 30min is until being completely dissolved in reaction, continuing stirring to heat up until when temperature goes up to 84 DEG C, starting to drip the pre-emulsion of 0.6g step A3 gained, time for adding is 2.5～3 hours;
A6. after described step A5 dropwises, continuing to drip the emulsified monomer of step A4 gained in described reactor one, time for adding is 1～1.5 hour, after dropwising, is incubated 30 minutes under 84 DEG C of conditions,
A7. in described step A6 products therefrom, add 0.002g initiator ammonium persulfate and 0.1g deionized water, be warming up to 90 DEG C and be incubated 1 hour,
A8. it is incubated after 1h reaction until described step A7 and is cooled to 65～70 DEG C immediately, dropping 0.001g tert-butyl hydroperoxide, time for adding is 10 minutes, when being then cooled to 56～60 DEG C, dropping sodium formaldehyde sulfoxylate 0.0015g, time for adding is 30 minutes, is cooled to 50 DEG C after dropwising, and namely prepares water-proof emulsion.
The preparation method of described adhesive specifically includes following steps:
B1. first add the water-proof emulsion of step A8 gained to reactor two, add 800 order dicalcium powders, be sufficiently stirred for 1 hour;
B2., after described step B1 stirs, add polyvinyl alcohol aqueous emulsion, stir 1 hour;
B3. after described step B2 stirs, add deionized water, stir 30min discharging, obtain adhesive to be prepared.
In the present embodiment, polyvinyl alcohol aqueous emulsion described in step B2 to be model be 2488 polyvinyl alcohol be dissolved as the aqueous emulsion that mass fraction is 17%～19%.
It should be noted that the volume ratio of described water-proof emulsion, dicalcium powder, polyvinyl alcohol aqueous emulsion and deionized water is 3～4:3～4:3:1～2.
The using method of a kind of timber aldehyde-free environment-friendly is water-fast high-strength adhesive, comprises the steps:
C1. before using, described adhesive and firming agent isocyanates are compared according to the quality of 1:10 and mix homogeneously;
C2. adopt artificial or machine roller coating method that the product after described step C1 gained mix homogeneously is coated on wood surface, and desirable gluing effect within 40 minutes, can be obtained 50 tons of pressure conjunctions.
Based on above-mentioned, adhesive environmental protection, adhesive strength prepared by the present invention are high, and resistance to water is better; And prepared adhesive is without formaldehyde, can at house decoration and artificial board etc. closely and extensive use in human lives's association area, environment and human body is substantially harmless, Environmental Safety.
The present invention adopts the emulsion that core-shell copolymerized polymerization is prepared from, timber finished product is prepared into through composite, emulsion adopts butyl acrylate and styrene to be nuclear monomer, react at 80-86 DEG C, adopt pre-emulsification seed dripping method, shell adopts styrene and methymethacrylate to be main, prepared adhesive and isocyanate curing agent fit in Bi-component adhesive, product has interior soft outer soft, structural strength high feature, with firming agent with the use of reaching D4 water protection standards, it is widely used in first timber pressing plate, the use of jigsaw, it is suitable for hardwood, the multiple timber and lumber standards of cork, and the preparation method technique of adhesive provided by the invention is simple, without " three wastes " discharge, with low cost.
Those of ordinary skill in the art will be appreciated that, above embodiments is intended merely to the explanation present invention, and it is not used as limitation of the invention, as long as in the spirit of the present invention, the change of embodiment described above, modification all will be dropped in scope of the presently claimed invention.
Claims (7)
1. the preparation method of the water-fast high-strength adhesive of timber aldehyde-free environment-friendly, it is characterised in that the preparation method of described adhesive includes the preparation method of water-proof emulsion and the preparation method of adhesive successively.
2. the preparation method of the water-fast high-strength adhesive of timber aldehyde-free environment-friendly according to claim 1, it is characterised in that the preparation method of described water-proof emulsion specifically includes following steps:
A1. in pre-emulsification still one, first adding the deionized water of 8 weight portions, add the N n-methylolacrylamide of 1 weight portion and the N-[2-(2-methyl-4-oxopentyl) of 0.28 weight portion, stirring 15min, until being completely dissolved;
A2. the solution after dissolving to described step A1 adds emulsifying agent, stirs 15min, slowly take out the monomer butyl acrylate adding 10 weight portions, abundant pre-emulsification;
A3. in pre-emulsified product abundant in step A2, it is initially charged the butyl acrylate of 13 weight portions, sequentially adds the acrylic acid of the styrene of 19 weight portions, the methymethacrylate of 2.8 weight portions and 1.1 weight portions, obtain pre-emulsion;
A4. in pre-emulsification still two, add the deionized water of 5 weight portions, add emulsifying agent, be then sequentially added into the acrylic acid of the styrene of 2.8 weight portions, the methymethacrylate of 2.2 weight portions and 1.1 weight portions, after fully emulsified emulsified monomer;
A5. the water of 34 weight portions is added to reactor one, when low whipping speed is warming up to 72 DEG C when being 30r/min, add the sodium bicarbonate of 0.06 weight portion, continue to add when stirring is warming up to 82 DEG C the initiator ammonium persulfate of 0.06 weight portion, 30min is until being completely dissolved in reaction, continuing stirring to heat up until when temperature goes up to 84 DEG C, starting to drip the pre-emulsion of the step A3 gained of 0.6 weight portion, time for adding is 2.5～3 hours;
A6. after described step A5 dropwises, continuing to drip the emulsified monomer of step A4 gained in described reactor one, time for adding is 1～1.5 hour, after dropwising, is incubated 30 minutes under 84 DEG C of conditions,
A7. in described step A6 products therefrom, add the initiator ammonium persulfate of 0.002 weight portion and the deionized water of 0.1 weight portion, be warming up to 90 DEG C and be incubated 1 hour,
A8. it is incubated after 1h reaction until described step A7 and is cooled to 65～70 DEG C immediately, drip the tert-butyl hydroperoxide of 0.001 weight portion, time for adding is 10 minutes, when being then cooled to 56～60 DEG C, drip the sodium formaldehyde sulfoxylate of 0.0015 weight portion, time for adding is 30 minutes, is cooled to 50 DEG C after dropwising, and namely prepares water-proof emulsion.
3. the preparation method of the water-fast high-strength adhesive of timber aldehyde-free environment-friendly according to claim 2, it is characterised in that the preparation method of described adhesive specifically includes following steps:
B1. first add the water-proof emulsion of step A8 gained to reactor two, add 800 order dicalcium powders, be sufficiently stirred for 1 hour;
B2., after described step B1 stirs, add polyvinyl alcohol aqueous emulsion, stir 1 hour;
B3. after described step B2 stirs, add deionized water, stir 30min discharging, obtain adhesive to be prepared.
4. the preparation method of the water-fast high-strength adhesive of timber aldehyde-free environment-friendly according to claim 3, it is characterised in that polyvinyl alcohol aqueous emulsion described in step B2 is model be 2488 polyvinyl alcohol be dissolved as the aqueous emulsion that mass fraction is 17%～19%.
5. the preparation method of the water-fast high-strength adhesive of timber aldehyde-free environment-friendly according to claim 3, it is characterised in that the volume ratio of described water-proof emulsion, dicalcium powder, polyvinyl alcohol aqueous emulsion and deionized water is 3～4:3～4:3:1～2.
6. the using method of the water-fast high-strength adhesive of timber aldehyde-free environment-friendly described in any one of claim 1-5, it is characterised in that comprise the steps:
C1. before using, described adhesive and firming agent are compared according to the quality of 1:10 and mix homogeneously;
C2. adopt artificial or machine roller coating method that the product after described step C1 gained mix homogeneously is coated on wood surface, and desirable gluing effect within 40 minutes, can be obtained 50 tons of pressure conjunctions.
7. the preparation method of the water-fast high-strength adhesive of timber aldehyde-free environment-friendly according to claim 6, it is characterised in that in described step C1, firming agent is isocyanates.
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| CN201610259037.5A CN105670535A (en) | 2016-04-25 | 2016-04-25 | Preparation method and application method of formaldehyde-free and environment-friendly type water-tolerant and high-strength adhesives |
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| CN108018006A (en) * | 2017-11-10 | 2018-05-11 | 山东凯源木业有限公司 | A kind of splicing adhesive |
| CN112724884A (en) * | 2020-12-28 | 2021-04-30 | 顶立新材料科技有限公司 | Styrene-acrylic emulsion plate alignment adhesive with long activation period and preparation method thereof |
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