CN102618198B - A kind of modified urea-formaldehyde glue and preparation method thereof - Google Patents
A kind of modified urea-formaldehyde glue and preparation method thereof Download PDFInfo
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- CN102618198B CN102618198B CN201210092888.7A CN201210092888A CN102618198B CN 102618198 B CN102618198 B CN 102618198B CN 201210092888 A CN201210092888 A CN 201210092888A CN 102618198 B CN102618198 B CN 102618198B
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Abstract
A kind of modified urea-formaldehyde glue and preparation method thereof, it relates to a kind of modified urea-formaldehyde glue and preparation method thereof.The present invention will solve existing urea-formaldehyde glue poor stability, the problem that the storage time is short.Urea-formaldehyde glue of the present invention is made up of formaldehyde, urea, trimeric cyanamide, p-methyl phenol, sodium cellulosate, ammoniacal liquor and polyvinyl alcohol.Preparation method is: one, take each component, is heated to 30 DEG C ~ 35 DEG C, regulates pH value, adds sodium cellulosate; Two, heat, add first part of urea, adjust pH value; Three, be warming up to 92 DEG C, adjust pH value, then insulation reaction; Four, adjust pH value, observing response terminal, adjust pH value to terminate reaction, add second part of urea, after mixing, be cooled to 70 DEG C, add the 3rd part of urea and add remaining ingredient again, cooling, adjust pH value, put glue and get final product.Urea-formaldehyde glue free formaldehyde content of the present invention is lower than 0.1%.Storage time is 2 months.The present invention is applied to urea-formaldehyde glue field.
Description
Technical field
The present invention relates to a kind of modified urea-formaldehyde glue and preparation method thereof.
Background technology
At present, be applied to the urea-formaldehyde glue of wood-processing industry, main raw material is formaldehyde and urea.Wherein formaldehyde content is very high, and formaldehyde has the feature of high volatility, and the gas of volatilization is comparatively strong to the pungency of people, and is harmful to health of human body.So study hypotoxic urea-formaldehyde glue to become current urgent problem.Come in, existing relevant report research, adopts novel modified urea-formaldehyde glue, free formaldehyde content can be made lower than 0.5%, but the stability that there is again glue is low, storage time is short, without precompressed in the course of processing, makes glued board quality low, thus increase labour intensity, be unfavorable for the raising of working efficiency, and existing urea-formaldehyde glue is in impregnation process, there is the danger of solidification, such as when impregnation, pH, lower than 4.6, just has the phenomenon of solidification.
Summary of the invention
The object of the invention is to solve existing urea-formaldehyde glue poor stability, the problem that the storage time is short, and a kind of modified urea-formaldehyde glue and preparation method thereof is provided.
A kind of modified urea-formaldehyde glue of the present invention be by ratio of weight and the number of copies by the mass percentage of 600 ~ 700 parts be the formaldehyde of 37%, the urea of 300 ~ 400 parts, the trimeric cyanamide of 35 ~ 45 parts, the p-methyl phenol of 3 ~ 7 parts, the sodium cellulosate of 3 ~ 7 parts, the mass percentage of 3 ~ 7 parts be that the ammoniacal liquor of 25% ~ 28% and the polyvinyl alcohol of 3 ~ 7 parts are made.
The preparation method of a kind of modified urea-formaldehyde glue of the present invention carries out according to following steps:
One, the mass percentage taking 600 ~ 700 parts is by ratio of weight and the number of copies the formaldehyde of 37%, the trimeric cyanamide of 35 ~ 45 parts, the p-methyl phenol of 3 ~ 7 parts, the sodium cellulosate of 3 ~ 7 parts, the mass percentage of 3 ~ 7 parts are the ammoniacal liquor of 25% ~ 28% and the polyvinyl alcohol of 3 ~ 7 parts;
Two, mass percentage step one taken be 37% formaldehyde add in reactor, heat temperature raising, when the pressure of boiler reaches 0.3MPa, when formaldehyde temperature in reactor reaches 30 DEG C ~ 35 DEG C, regulate formaldehyde pH to 7.5 ~ 8.0 with the caustic soda solution that concentration is 25% ~ 30%, then add the sodium cellulosate that step one takes;
Three, the formaldehyde temperature be heated in reactor is continued when reaching 36 DEG C ~ 40 DEG C, formaldehyde pH to 8.0 is regulated with the caustic soda solution that concentration is 25% ~ 30%, add the urea of 200 ~ 220 weight parts, mix, obtain just mixed liquid, employing concentration is first mixed liquid pH to 6.3 ~ 6.5 of caustic soda solution adjustment of 25% ~ 30%;
Four, continuing reacting by heating still is 72 DEG C ~ 78 DEG C to temperature, heating is stopped when boiler pressure is 1.5 ~ 2.0MPa, 92 DEG C are warming up to by reactor self-heat generation, adopt again concentration be 25% ~ 30% caustic soda solution regulate pH value of solution to 6.3 ~ 6.5 of solution in reactor, insulation reaction 30 ~ 40 minutes, obtains mixed solution;
Five, adopt concentration be 25% ~ 28% pH of mixed to 4.8 ~ 5.0 that obtain of ammonium chloride solution regulating step four, mixed solution is added drop-wise to when observing to reaction end in 8 ~ 10 DEG C of water, pH of mixed to 6.7 ~ 7.2 are regulated again with the caustic soda solution that concentration is 25% ~ 30%, add the urea of 90 ~ 100 weight parts again, be uniformly mixed 10 ~ 20 minutes, mixed solution is cooled to 70 DEG C, then the urea of 10 ~ 20 weight parts is added, the p-methyl phenol that step one takes, ammoniacal liquor and trimeric cyanamide, after stirring, when mixed solution being cooled to 40 DEG C, mixed solution pH value to 7.5 ~ 8.5 are regulated again with the caustic soda solution that concentration is 25% ~ 30%, put glue, obtain urea-formaldehyde glue, described reaction reaches terminal and refers to that recording viscosity with painting-4 glasss reaches 25 ~ 30 seconds/25 DEG C.
Beneficial effect of the present invention:
The ammoniacal liquor added in urea-formaldehyde glue of the present invention can reduce formaldehyde content further, and the p-methyl phenol added can make glue can increase the heated aqueous of glue further, makes content of free aldehyde be down to very low value, and urea-formaldehyde glue Free-formaldehyde content of the present invention is lower than 0.1%.
Sodium cellulosate in urea-formaldehyde glue of the present invention can improve the tack of glue, improves the water-soluble of glue, urea-formaldehyde glue is reacted in the environment of 8 DEG C ~ 10 DEG C, improves urea-formaldehyde glue stability; And glue can be made to store 2 months, more existing urea-formaldehyde glue stores 1 month to be compared and is significantly improved.Urea-formaldehyde glue of the present invention is in the actual course of processing, add polyvinyl alcohol, the precompressed of glued board is improved, compare at present without the glued board of precompressed, the quality of glued board can be improved, owing to carrying out precompressed in advance, therefore, can working efficiency be saved, avoid, because there is the problems such as skew when suppressing glued board, affecting working efficiency.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: a kind of modified urea-formaldehyde glue of present embodiment, be by ratio of weight and the number of copies by the mass percentage of 600 ~ 700 parts be the formaldehyde of 37%, the urea of 300 ~ 400 parts, the trimeric cyanamide of 35 ~ 45 parts, the p-methyl phenol of 3 ~ 7 parts, the sodium cellulosate of 3 ~ 7 parts, the mass percentage of 3 ~ 7 parts be that the ammoniacal liquor of 25% ~ 28% and the polyvinyl alcohol of 3 ~ 7 parts are made.
The ammoniacal liquor added in the urea-formaldehyde glue of present embodiment can reduce formaldehyde content further, the p-methyl phenol added can make glue can increase the heated aqueous of glue further, make content of free aldehyde be down to very low value, present embodiment urea-formaldehyde glue Free-formaldehyde content is lower than 0.1%.
Sodium cellulosate in the urea-formaldehyde glue of present embodiment can improve the tack of glue, improves the water-soluble of glue, urea-formaldehyde glue is reacted in the environment of 8 DEG C ~ 10 DEG C, improves urea-formaldehyde glue stability; And glue can be made to store 2 months, more existing urea-formaldehyde glue stores 1 month to be compared and is significantly improved.The urea-formaldehyde glue of present embodiment is in the actual course of processing, add polyvinyl alcohol, the precompressed of glued board is improved, compare at present without the glued board of precompressed, the quality of glued board can be improved, owing to carrying out precompressed in advance, therefore, can working efficiency be saved, avoid, because there is the problems such as skew when suppressing glued board, affecting working efficiency.
Embodiment two: present embodiment and embodiment one unlike: urea-formaldehyde glue by weight by the mass percentage of 666 parts be the formaldehyde of 37%, the urea of 333 parts, the trimeric cyanamide of 40 parts, the p-methyl phenol of 5 parts, the sodium cellulosate of 5 parts, the mass percentage of 5 parts be that the ammoniacal liquor of 25% ~ 28% and the polyvinyl alcohol of 5 parts form.Other is identical with embodiment one.
Embodiment three: the preparation method of a kind of modified urea-formaldehyde glue of present embodiment carries out according to following steps: the mass percentage one, taking 600 ~ 700 parts is by ratio of weight and the number of copies the formaldehyde of 37%, the trimeric cyanamide of 35 ~ 45 parts, the p-methyl phenol of 3 ~ 7 parts, the sodium cellulosate of 3 ~ 7 parts, the mass percentage of 3 ~ 7 parts are the ammoniacal liquor of 25% ~ 28% and the polyvinyl alcohol of 3 ~ 7 parts;
Two, mass percentage step one taken be 37% formaldehyde add in reactor, by boiler heat temperature raising, when the pressure of boiler reaches 0.3MPa, when formaldehyde temperature in reactor reaches 30 DEG C ~ 35 DEG C, regulate formaldehyde pH to 7.5 ~ 8.0 with the caustic soda solution that concentration is 25% ~ 30%, then add the sodium cellulosate that step one takes;
Three, the formaldehyde temperature be heated in reactor is continued when reaching 36 DEG C ~ 40 DEG C, formaldehyde pH to 8.0 is regulated with the caustic soda solution that concentration is 25% ~ 30%, add the urea of 200 ~ 220 weight parts, mix, obtain just mixed liquid, employing concentration is first mixed liquid pH to 6.3 ~ 6.5 of caustic soda solution adjustment of 25% ~ 30%;
Four, continuing reacting by heating still is 72 DEG C ~ 78 DEG C to temperature, heating is stopped when boiler pressure is 1.5 ~ 2.0MPa, 92 DEG C are warming up to by reactor self-heat generation, adopt again concentration be 25% ~ 30% caustic soda solution regulate pH value of solution to 6.3 ~ 6.5 of solution in reactor, insulation reaction 30 ~ 40 minutes, obtains mixed solution;
Five, adopt concentration be 25% ~ 28% pH of mixed to 4.8 ~ 5.0 that obtain of ammonium chloride solution regulating step four, mixed solution is added drop-wise to when observing to reaction end in 8 ~ 10 DEG C of water, pH of mixed to 6.7 ~ 7.2 are regulated again with the caustic soda solution that concentration is 25% ~ 30%, add the urea of 90 ~ 100 weight parts again, be uniformly mixed 10 ~ 20 minutes, mixed solution is cooled to 70 DEG C, then the urea of 10 ~ 20 weight parts is added, the p-methyl phenol that step one takes, ammoniacal liquor and trimeric cyanamide, after stirring, when mixed solution being cooled to 40 DEG C, mixed solution pH value to 7.5 ~ 8.5 are regulated again with the caustic soda solution that concentration is 25% ~ 30%, put glue, obtain urea-formaldehyde glue, described reaction reaches terminal and refers to that recording viscosity with painting-4 glasss reaches 25 ~ 30 seconds/25 DEG C.
The ammoniacal liquor added in the urea-formaldehyde glue of present embodiment can reduce formaldehyde content further, the p-methyl phenol added can make glue can increase the heated aqueous of glue further, make content of free aldehyde be down to very low value, present embodiment urea-formaldehyde glue Free-formaldehyde content is lower than 0.1%.
Sodium cellulosate in the urea-formaldehyde glue of present embodiment can improve the tack of glue, improves the water-soluble of glue, urea-formaldehyde glue is reacted in the environment of 8 DEG C ~ 10 DEG C, improves urea-formaldehyde glue stability; And glue can be made to store 2 months, more existing urea-formaldehyde glue stores 1 month to be compared and is significantly improved.The urea-formaldehyde glue of present embodiment is in the actual course of processing, add polyvinyl alcohol, the precompressed of glued board is improved, compare at present without the glued board of precompressed, the quality of glued board can be improved, owing to carrying out precompressed in advance, therefore, can working efficiency be saved, avoid, because there is the problems such as skew when suppressing glued board, affecting working efficiency.
Specifically embodiment four: present embodiment and embodiment three unlike: the formaldehyde temperature in the reactor described in step 2 is 32 DEG C ~ 34 DEG C.Other step and parameter identical with step 3.
Specifically embodiment five: present embodiment and embodiment three to four unlike: the mass percentage taking 666 parts by ratio of weight and the number of copies described in step one is the formaldehyde of 37%, the urea of 333 parts, the trimeric cyanamide of 40 parts, the p-methyl phenol of 5 parts, the sodium cellulosate of 5 parts, the mass percentage of 5 parts are the ammoniacal liquor of 25% ~ 28% and the polyvinyl alcohol of 5 parts.Other step and parameter identical with step 3 to four.
Specifically embodiment six: one of present embodiment and embodiment three to five unlike: the pH described in step 2 is 7.8.Other step and parameter identical with one of step 3 to five.
Specifically embodiment seven: one of present embodiment and embodiment three to six unlike: the reacting by heating still described in step 4 to temperature is 74 DEG C ~ 76 DEG C.Other step and parameter identical with one of step 3 to six.
Specifically embodiment eight: one of present embodiment and embodiment three to seven were unlike the insulation reaction described in step 4 35 minutes.Other step and parameter identical with one of step 3 to seven.
Specifically embodiment nine: one of present embodiment and embodiment three to eight unlike: when being added drop-wise to by mixed solution described in step 5 is observed to reaction end in 8 ~ 10 DEG C of water, then with concentration be 25% ~ 30% caustic soda solution regulate pH of mixed to 7.0.Other step and parameter identical with one of step 3 to eight.
Specifically embodiment ten: one of present embodiment and embodiment three to eight unlike: described in step 5 mixed solution is cooled to 40 DEG C time, then with concentration be 25% ~ 30% caustic soda solution regulate mixed solution pH value to 7.8 ~ 8.2.Other step and parameter identical with one of step 3 to eight.
By following verification experimental verification effect of the present invention:
Test
The preparation method of a kind of modified urea-formaldehyde glue of this test carries out according to following steps:
One, the polyvinyl alcohol of the formaldehyde of the concentration 37% of 666kg, the trimeric cyanamide of 40kg, the p-methyl phenol of 5kg, the sodium cellulosate of 5kg and 5kg is taken by ratio of weight and the number of copies;
Two, concentration step one taken be 37% formaldehyde add in reactor, heat temperature raising, when reactor pressure reaches 0.3Mpa, when temperature is 35 DEG C, regulates formaldehyde pH to 8.0 with the caustic soda solution that concentration is 25%, then adds the sodium cellulosate that step one takes;
Three, continuation reacting by heating still to 40 DEG C, after regulating pH to 8.0, adds the urea of 214kg first, mixes with the caustic soda solution that concentration is 25%, obtains just mixed liquid, and employing concentration is the caustic soda solution adjustment just mixed liquid pH to 6.5 of 25%;
Four, continuing reacting by heating still is 75 DEG C to temperature, stops heating, be warming up to 92 DEG C by self-heat generation when pressure is 1.8Mpa, and employing concentration is the caustic soda solution adjustment pH to 6.5 of 25%, and insulation reaction 30 minutes, obtains mixed solution;
Five, adopt mass percentage be 28% the pH of mixed to 5.0 that obtains of ammonium chloride solution regulating step four, observation reaches reaction end, record viscosity with painting-4 glasss and reach 25 ~ 30 seconds/8 DEG C, pH to 7.2 is regulated again with the caustic soda solution that concentration is 25%, add the urea of 99kg again, be uniformly mixed 15 minutes, mixed solution is cooled to 70 DEG C, then the urea of 20kg is added, the p-methyl phenol that step one takes and trimeric cyanamide, after stirring, when mixed solution being continued be cooled to 40 DEG C, mixed solution pH value to 8.0 is regulated with the caustic soda solution that concentration is 25%, put glue, obtain urea-formaldehyde glue.
The urea-formaldehyde glue that this test obtains can deposit 2 months, and the urea-formaldehyde glue shelf-time is 2 months, than existing increase by 1 times; The urea-formaldehyde glue Free-formaldehyde content that this test obtains is lower than 0.1%.The enough environment at 8 DEG C ~ 10 DEG C of this test urea-formaldehyde glue react.Environment reacts.
Claims (10)
1. a modified urea-formaldehyde glue, it is characterized in that urea-formaldehyde glue be by ratio of weight and the number of copies by the mass percentage of 600 ~ 700 parts be the formaldehyde of 37%, the urea of 300 ~ 400 parts, the trimeric cyanamide of 35 ~ 45 parts, the p-methyl phenol of 3 ~ 7 parts, the sodium cellulosate of 3 ~ 7 parts, the mass percentage of 3 ~ 7 parts be that the ammoniacal liquor of 25% ~ 28% and the polyvinyl alcohol of 3 ~ 7 parts are made.
2. a kind of modified urea-formaldehyde glue according to claim 1, it is characterized in that urea-formaldehyde glue by weight by the mass percentage of 666 parts be the formaldehyde of 37%, the urea of 333 parts, the trimeric cyanamide of 40 parts, the p-methyl phenol of 5 parts, the sodium cellulosate of 5 parts, the mass percentage of 5 parts be that the ammoniacal liquor of 25% ~ 28% and the polyvinyl alcohol of 5 parts form.
3. the preparation method of a kind of modified urea-formaldehyde glue as claimed in claim 1, is characterized in that a kind of preparation method of modified urea-formaldehyde glue carries out according to following steps:
One, the mass percentage taking 600 ~ 700 parts is by ratio of weight and the number of copies the formaldehyde of 37%, the trimeric cyanamide of 35 ~ 45 parts, the p-methyl phenol of 3 ~ 7 parts, the sodium cellulosate of 3 ~ 7 parts, the mass percentage of 3 ~ 7 parts are the ammoniacal liquor of 25% ~ 28% and the polyvinyl alcohol of 3 ~ 7 parts;
Two, mass percentage step one taken be 37% formaldehyde add in reactor, by boiler heat temperature raising, when the pressure of boiler reaches 0.3MPa, when formaldehyde temperature in reactor reaches 30 DEG C ~ 35 DEG C, regulate formaldehyde pH to 7.5 ~ 8.0 with the caustic soda solution that concentration is 25% ~ 30%, then add the sodium cellulosate that step one takes;
Three, the formaldehyde temperature be heated in reactor is continued when reaching 36 DEG C ~ 40 DEG C, formaldehyde pH to 8.0 is regulated with the caustic soda solution that concentration is 25% ~ 30%, add the urea of 200 ~ 220 weight parts, mix, obtain just mixed liquid, employing concentration is first mixed liquid pH to 6.3 ~ 6.5 of caustic soda solution adjustment of 25% ~ 30%;
Four, continuing reacting by heating still is 72 DEG C ~ 78 DEG C to temperature, heating is stopped when boiler pressure is 1.5 ~ 2.0MPa, 92 DEG C are warming up to by reactor self-heat generation, adopt again concentration be 25% ~ 30% caustic soda solution regulate pH value of solution to 6.3 ~ 6.5 of solution in reactor, insulation reaction 30 ~ 40 minutes, obtains mixed solution;
Five, adopt concentration be 25% ~ 28% pH of mixed to 4.8 ~ 5.0 that obtain of ammonium chloride solution regulating step four, mixed solution is added drop-wise to when observing to reaction end in 8 ~ 10 DEG C of water, pH of mixed to 6.7 ~ 7.2 are regulated again with the caustic soda solution that concentration is 25% ~ 30%, add the urea of 90 ~ 100 weight parts again, be uniformly mixed 10 ~ 20 minutes, mixed solution is cooled to 70 DEG C, then the urea of 10 ~ 20 weight parts is added, the p-methyl phenol that step one takes, ammoniacal liquor and trimeric cyanamide, after stirring, when mixed solution being cooled to 40 DEG C, mixed solution pH value to 7.5 ~ 8.5 are regulated again with the caustic soda solution that concentration is 25% ~ 30%, put glue, obtain urea-formaldehyde glue, described reaction reaches terminal and refers to that recording viscosity with painting-4 glasss reaches 25 ~ 30 seconds/25 DEG C.
4. the preparation method of a kind of modified urea-formaldehyde glue according to claim 3, is characterized in that described caustic soda solution is NaOH solution.
5. the preparation method of a kind of modified urea-formaldehyde glue according to claim 3, is characterized in that the mass percentage taking 666 parts by ratio of weight and the number of copies described in step one is the formaldehyde of 37%, the urea of 333 parts, the trimeric cyanamide of 40 parts, the p-methyl phenol of 5 parts, the sodium cellulosate of 5 parts, the mass percentage of 5 parts are the ammoniacal liquor of 25% ~ 28% and the polyvinyl alcohol of 5 parts.
6. the preparation method of a kind of modified urea-formaldehyde glue according to claim 3, is characterized in that the pH described in step 2 is 7.8.
7. the preparation method of a kind of modified urea-formaldehyde glue according to claim 3, is characterized in that reacting by heating still to the temperature described in step 4 is 74 DEG C ~ 76 DEG C.
8. the preparation method of a kind of modified urea-formaldehyde glue according to claim 3, is characterized in that insulation reaction described in step 4 35 minutes.
9. the preparation method of a kind of modified urea-formaldehyde glue according to claim 3, when it is characterized in that being added drop-wise to by mixed solution described in step 5 is observed to reaction end in 8 ~ 10 DEG C of water, then regulates pH of mixed to 7.0 with the caustic soda solution that concentration is 25% ~ 30%.
10. the preparation method of a kind of modified urea-formaldehyde glue according to claim 3, it is characterized in that described in step 5 mixed solution is cooled to 40 DEG C time, then with concentration be 25% ~ 30% caustic soda solution regulate mixed solution pH value to 7.8 ~ 8.2.
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| CN103666349A (en) * | 2013-11-22 | 2014-03-26 | 黑龙江大学 | Anti-aging modified urea-formaldehyde glue and preparation method thereof |
| CN103555241B (en) * | 2013-11-22 | 2015-02-04 | 黑龙江大学 | Flame-retardant modified urea-formaldehyde glue and application thereof |
| CN103555240B (en) * | 2013-11-22 | 2014-12-17 | 黑龙江大学 | Modified urea-formaldehyde glue with musk smell |
| CN104592911B (en) * | 2015-02-09 | 2016-06-29 | 金思思 | A kind of plywood adhesive composition and preparation technology thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101200549A (en) * | 2007-12-04 | 2008-06-18 | 中国林业科学研究院木材工业研究所 | Method for preparing modified urea-formaldehyde resin powder material |
| CN101265314A (en) * | 2008-04-30 | 2008-09-17 | 北京化工大学 | Environmental protection urea-formaldehyde resin and preparation method thereof |
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| CN101200549A (en) * | 2007-12-04 | 2008-06-18 | 中国林业科学研究院木材工业研究所 | Method for preparing modified urea-formaldehyde resin powder material |
| CN101265314A (en) * | 2008-04-30 | 2008-09-17 | 北京化工大学 | Environmental protection urea-formaldehyde resin and preparation method thereof |
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