CN103319674A - Preparation method for natural vegetable gum-modified urea-formaldehyde resin - Google Patents
Preparation method for natural vegetable gum-modified urea-formaldehyde resin Download PDFInfo
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- CN103319674A CN103319674A CN2013102648014A CN201310264801A CN103319674A CN 103319674 A CN103319674 A CN 103319674A CN 2013102648014 A CN2013102648014 A CN 2013102648014A CN 201310264801 A CN201310264801 A CN 201310264801A CN 103319674 A CN103319674 A CN 103319674A
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Abstract
The invention discloses a preparation method for natural vegetable gum-modified urea-formaldehyde resin. The preparation method comprises a vegetable gum resin synthesis step and a vegetable gum-modified urea-formaldehyde resin synthesis step. The vegetable gum resin synthesis step involves the following raw materials in percentage by weight: 85 to 91 percent of water, 2.5 to 8 percent of vegetable gum, 0.1 to 0.2 percent of triethanolamine, 1.5 to 4 percent of 39.540.5wt% glyoxal solution, 0.1 to 0.5 percent of anhydrous sodium carbonate, 1 to 3 percent of urea, 2 to 6 percent of 36.5-37.4wt% formaldehyde solution, 1 to 4 percent of 25wt% ammonia water and 0.2 to 1 percent of melamine. The preparation method has the advantages that the urea-formaldehyde resin is modified by the natural vegetable gum, so that stable loop structures are introduced into resin molecular structures, the toughness of the urea-formaldehyde resin is improved, the number of ether bonds is reduced, and the water resistance of the resin is improved. The resin is fully polycondensated; the water solubility is high; the activity of hydroxymethyl during high-temperature curing is enhanced; the curing of the resin is promoted; the resin density is increased.
Description
Technical field
The present invention relates to a kind of preparation method of vegetable jelly modified urea-formaldehyde resin, particularly Fibreboard Production belongs to the adhesive of artificial board field with environment-friendly urea-formaldehyde resin and preparation method thereof.
Background technology
Medium and high density fibre panel is owing to its excellent performance, being convenient to processing, the characteristics such as moderate, and the green grass or young crops that always is subject to people is paid attention to.Along with scientific-technical progress, the derivative series product of fiberboard, the continuous appearance of deep processing kind and perfect, all kinds of fiberboards will be applied in the national economy every field more and more widely.
Fibreboard Production be unable to do without tackiness agent.At present, urea-formaldehyde resin adhesive accounts for Fibreboard Production and sticks with glue more than 90% of agent total amount, is the kind of consumption maximum in the tackiness agent.Urea-formaldehyde resin has the incomparable advantage of other resin, mainly be that its raw material is sufficient, cheap, that cost is minimum in the synthetic resins, and behind the resin solidification high, the glue-line of the transparency without color, can not pollute by the plate face of cementing thing, good water solubility easily is modulated to needed appropriate viscosity and concentration.But urea-formaldehyde resin also has some obvious shortcomings, poor except ageing resistance, hot water resistance is poor, can not be as outdoor wood-based plate with the glue, its fatal shortcoming is that the wood-based panel product that glueds joint exists the formaldehyde release And Spread of Solute.
The formaldehyde of wood-based plate discharges, and mainly comes from urea-formaldehyde resin.Usually, reduction of formaldehyde emission must be from reducing glue Free-formaldehyde content and improving the aspects such as resin microtexture.Improve the synthesis technique of urea-formaldehyde resin, reduce mol ratio, adding properties-correcting agent and formaldehyde-trapping agent etc. is the method for commonly using.But the reduction of mol ratio will cause the urea-formaldehyde resin cross-linking density to descend, and tack reduces, and prolong set time, and shorten storage period, and the mechanical property variation of wood-based plate is difficult to satisfy service requirements; The price of properties-correcting agent and formaldehyde-trapping agent is generally all relatively expensive, and can make increases the Wood-based Panel Production cost.Therefore, in order to produce the environmental protection urea-formaldehyde resin of low burst size of methanal, not affecting again other performance of resin simultaneously, improve the synthesis technique of urea-formaldehyde resin, is a kind of both economical feasible method.Vegetable jelly is widely used in papermaking, building, finishing, petrochemical complex, textile industry with its polymer characteristics, but rarely has report in the application of adhesive of artificial board industry.
The patent of application number 201010524120.3 relates to a kind of preparation method of the vegetable jelly toughener for papermaking, it is characterized in that: with vegetable jelly, sesbania gum, guar gum, water glass, after hydration, carry out cross reaction and crosslinking reaction with sodium tetraborate, trimeric cyanamide acetaldehyde resin, vulkacit H again, namely prepare the vegetable jelly toughener.Product can become the additive for papermaking of harmless degraded in physical environment.
The patented invention of application number 201210442657.4 a kind of environment-friendly type building tackiness agent, specifically adopt microcapsulary that linking agent is carried out modification, make it under dry powder, with the natural plant blend crosslinking reaction not occur, linking agent discharges and plant gum powder generation crosslinking reaction when being dissolved in water, solve the defective that natural plant prepares the tackiness agent poor water resistance, had the advantages such as stronger water-soluble, water tolerance, cohesiveness, environmental protection.
The patent of application number 201110421433.0 discloses a kind of modified plant gum and preparation method thereof.Add organosilane monomer, catalytic promoter and plant monomer in vegetable jelly, the outward appearance of the modified plant gum that is made by this preparation method is milky white liquid, is used for the preparation of emulsion paint.
The patent Introduction of application number 201210423102.5 be host with vegetable jelly, a kind of non-formaldehyde wood adhesive of tributyl phosphate or vinyl acetate modified preparation, solved present low without the aldehyde Joint strength, the defective of water-fast difference.
In sum, the report that is used for the Fibreboard Production field with the natural plant modified urea-formaldehyde resin seldom, natural plant is used for wood working industry and has good prospect.Follow people to improving constantly that indoor environment requires, ultra-low formaldehyde discharges even the high-end fiberboard of formaldehydeless release will become following main product.Vegetable jelly modified urea-formaldehyde resin of the present invention has ultra-low formaldehyde content, and vegetable jelly molecule and the graft copolymerization of urea aldehyde molecule are fit to the compacting environment protection pressed-fibre board, are particularly useful for suppressing the high intensity low density fiberboard.
Summary of the invention
The fragility, the formaldehyde that the objective of the invention is for conventional modified urea-formaldehyde resin discharge shortcoming high, poor water resistance, and a kind of preparation method of vegetable jelly modified urea-formaldehyde resin is provided.
Principle of the present invention is to utilize novel modified natural vegetable jelly blend graft urea-formaldehyde resin, and the methylol group content in the control resin is introduced cyclic group, reduces the methylene ether linkage content, improves the microtexture of resin.The content of free aldehyde of resin is low, and cross-linking density is high during curing, and the physical and chemical index of pressed density plate is substantially constant, and burst size of methanal is ultralow.
For realizing purpose of the present invention, natural plant modified urea-formaldehyde resin of the present invention is comprised of the synthesis step of vegetable jelly resin and the synthesis step of vegetable jelly modified urea-formaldehyde resin; Wherein the raw material of the synthesis step of vegetable jelly resin is by weight percentage: water 85-91%, vegetable jelly 2.5-8%, trolamine 0.1-0.2%, the glyoxal solution 1.5-4% of mass concentration 39.5-40.5%, anhydrous sodium carbonate 0.1-0.5%, urea 1-3%, the formaldehyde solution 2-6% of mass concentration 36.5-37.4%, the ammoniacal liquor 1-4% of mass concentration 25%, trimeric cyanamide 0.2-1%;
1) the synthetic concrete steps of vegetable jelly resin are as follows:
A, slowly add vegetable jelly in the water, and stir;
B, vegetable jelly dissolve rear adding trolamine fully, survey pH=8.5-9.0, are warming up to 55-60 ℃ of insulation, reach 800-1200mPas(25 ℃ to viscosity);
C, reach add after the viscosity pH adjusting agent to pH be 5.0-6.0, add glyoxal solution, then add the urea of anhydrous sodium carbonate and 0.5-1.5%, insulation 1-2h;
D, adding formaldehyde solution, ammoniacal liquor and trimeric cyanamide;
E, be warming up to 80-85 ℃, be incubated to viscosity reach 1000-1600mPas(25 ℃), then begin cooling;
F, when being cooled to 40-45 ℃, add pH adjusting agent to pH=7.0-7.5, add the urea of 0.5-2.5%, insulation 20-30min, rear discharging stirs;
The raw material of vegetable jelly modified urea-formaldehyde resin synthesis step is by weight percentage: the vegetable jelly resin 45-60% that step 1) is synthetic, the formaldehyde solution 20-38% of mass concentration 36.5-37.4%, urotropine 0.1-0.3%, urea 15-30%, trimeric cyanamide 0.5-2%;
The concrete steps that the vegetable jelly modified urea-formaldehyde resin synthesizes are as follows:
G, formaldehyde solution, urotropine mixed transfer pH to 7.0-7.5, add first urea, wherein formaldehyde is 2.0-3.0:1 with the ratio of the mole number of first urea;
H, be warmed up to 85-95 ℃, insulation 30-50min;
I, adding pH adjusting agent continue reaction 80-100min to pH to 4.5-5.5;
J, add pH adjusting agent to pH to 5.2-5.6, add second batch urea, the mole number that makes the formaldehyde that adds among the step G is 1.5-1.9:1 with the ratio of the total mole number of two batches of urea, continues to react to viscosity 100-300mPas(25 ℃);
K, add pH adjusting agent and transfer pH to 7.0-7.5, add the urea of surplus, the mole number that makes the formaldehyde that adds among the step G is 0.8-1.4:1 with the ratio of the total mole number of three batches of urea, begins cooling;
L, be cooled to 65-75 ℃, add trimeric cyanamide, insulation 10-20min;
M, the synthetic vegetable jelly resin of adding step 1) stir 15-30min, are cooled to 35-40 ℃, add pH adjusting agent to pH to 7.5-8.5 discharging and namely get the vegetable jelly modified urea-formaldehyde resin.
Such scheme is more preferably:
Described vegetable jelly is one or more in sesbania gum, guar gum, xanthan gum, the Viscogum BE;
PH adjusting agent among described step F, J, K, the M is one or more in ammoniacal liquor, sodium hydroxide solution or the trolamine.
PH adjusting agent among described step C, the I is selected from one or more in formic acid, oxalic acid, citric acid, the tartrate.
The formaldehyde that adds among the described step G is 2.24:1 with the ratio of the mole number of first urea, and it is 50 ℃ that urea adds temperature.
Under the described step J condition, the reaction times is 80-100min, and reaction solution viscosity should be controlled 150-250mPas(25 ℃).
Among the described step J, the formaldehyde that adds among the step G is 1.78:1 with the ratio of the total mole number of two batches of urea, and it is 90 ℃ that urea adds temperature.
In the described step K, the formaldehyde that adds among the step G is 0.82:1 with the ratio of the total mole number of three batches of urea, and it is 85 ℃ that urea adds temperature.
The advantage of the inventive method is: by the natural plant modified urea-formaldehyde resin, make the stable ring texture of introducing in the resinous molecular structure, improved the toughness of urea-formaldehyde resin, reduced the quantity of ehter bond, improved the water tolerance of resin.The resin polycondensation is more abundant, good water solubility, and the increased activity of methylol during hot setting promotes the curing of resin, strengthens the degree of compactness of resin.
Embodiment
Describe the present invention in detail below by embodiment, it should be understood that these embodiment only are used for the purpose of illustration, never limit protection scope of the present invention.It will be understood by those skilled in the art that and do not departing under spirit of the present invention and the periphery and can make amendment or replace the details of technical solution of the present invention and form, but these modifications or replace all fall within the scope of protection of the present invention.
[embodiment]
The composition of raw materials of table 1 embodiment one
Annotate: F and U represent respectively the formaldehyde solution that adds and the weight number of urea, U
1-U
3Represent respectively the weight number of the urea of first to the 3rd batch of adding, f and u represent respectively the mole number of formaldehyde and urea, u
1-u
3The mole number that represents respectively the urea of first to the 3rd batch of adding, f/u represent the mole number of formaldehyde and the ratio of the mole number of urea.
Concrete reactions steps is as follows:
1) the vegetable jelly resin is synthetic:
The water that A, adding measure is opened and is stirred, and then slowly adds and measures guar gum, water flushing coil pipe and still wall;
B, add trolamine after the dissolving fully, survey pH=8.5-9.0, begin to heat up, be warming up to 60 ℃ of insulations, every the 10min test once, reach 1000-1200mPas to viscosity;
C, reach that to transfer pH after the viscosity be 5.5-6.0, add immediately glyoxal solution, then add anhydrous sodium carbonate and urea, insulation 1.5h transfers pH=6.5-7.0;
D, adding formaldehyde solution F1, ammoniacal liquor and trimeric cyanamide;
E, continue to be warming up to 85 ℃, insulation 30min every the 10min test once, reaches 1200-1600mPas(25 ℃ to viscosity), then begin cooling;
F, when being cooled to 40-45 ℃, surveying pH and also transfer pH=7.0-7.5, add urea, be incubated 20 minutes, rear discharging stirs.
2) urea-formaldehyde resin is synthetic:
G, with the formaldehyde solution F2 of metering, add urotropine and transfer pH to 7.0-7.5, add U1, the mole number of formaldehyde is 2.24:1 with the ratio of the mole number of a urea;
H, be warmed up to 85 ℃, insulation 30-50min;
I, transfer pH to 4.5-5.0 with formic acid solution, reaction 80-100min;
J, transfer pH to 5.2-5.4 with sodium hydroxide solution, add U2, the mole number that makes the formaldehyde that adds among the step G is 1.78:1 with the ratio of the total mole number of two batches of urea, reacts to viscosity 200-300mPas(25 ℃);
K, transfer pH to 7.0-7.2 with sodium hydroxide solution, add U3, the mole number that makes the formaldehyde that adds among the step G is 0.82:1 with the ratio of the total mole number of three batches of urea, begins cooling;
L, be cooled to 65 ℃, add trimeric cyanamide, insulation 10-20min;
M, the synthetic vegetable jelly resin of adding step 1) stir 20min, are cooled to about 35-40 ℃, transfer pH to 7.5-8.0 discharging with sodium hydroxide solution.
The quality index of gained resin:
Solids content: 44-47%
PH value: 7.5-8.0
Viscosity (25 ℃): 120-180mPas
Curing speed: 110-140s
Free formaldehyde content: 0.01%
Storage period:＞30 days
[embodiment two]
The composition of raw materials of table 2 embodiment two:
Annotate: F and U represent respectively the formaldehyde solution that adds and the weight number of urea, U
1-U
3Represent respectively the weight number of the urea of first to the 3rd batch of adding, f and u represent respectively the mole number of formaldehyde and urea, u
1-u
3The mole number that represents respectively the urea of first to the 3rd batch of adding, f/u represent the mole number of formaldehyde and the ratio of the mole number of urea.
Concrete reactions steps is as follows:
1) the vegetable jelly resin is synthetic:
The water that A, adding measure is opened and is stirred, and then slowly adds and measures guar gum, water flushing coil pipe and still wall;
B, add trolamine after the dissolving fully, survey pH=8.5-9.0, begin to heat up, be warming up to 60 ℃ of insulations, every the 10min test once, reach 800-1000mPas to viscosity;
C, reach that to transfer pH after the viscosity be 5.5-6.0, add immediately glyoxal solution, then add anhydrous sodium carbonate and urea, insulation 1-2h transfers pH=6.5-7.0;
D, adding formaldehyde solution F1, ammoniacal liquor and trimeric cyanamide;
E, continue to be warming up to 85 ℃, insulation 30min every the 10min test once, reaches 1100-1500mPas(25 ℃ to viscosity), then begin cooling;
F, when being cooled to 40-45 ℃, surveying pH and also transfer pH=7.0-7.5, add urea, be incubated 20 minutes, rear discharging stirs.
2) urea-formaldehyde resin is synthetic:
G, with the formaldehyde solution F2 of metering, add urotropine and transfer pH to 7.0-7.5, add U1, the mole number of formaldehyde is 2.18:1 with the ratio of the mole number of a urea;
H, be warmed up to 85 ℃, insulation 30-50min;
I, transfer pH to 4.5-5.0 with oxalic acid solution, reaction 80-100min;
J, transfer pH to 5.2-5.4 with sodium hydroxide solution, add U2, the mole number that makes the formaldehyde that adds among the step G is 1.66:1 with the ratio of the total mole number of two batches of urea, reacts to viscosity 100-200mPas(25 ℃);
K, transfer pH to 7.0-7.2 with sodium hydroxide solution, add U3, the mole number that makes the formaldehyde that adds among the step G is 0.96:1 with the ratio of the total mole number of three batches of urea, begins cooling;
L, be cooled to 65 ℃, add trimeric cyanamide, insulation 10-20min;
M, the synthetic vegetable jelly resin of adding step 1) stir 20min, are cooled to 35-40 ℃, transfer pH to 7.5-8.0 discharging with sodium hydroxide solution.
The quality index of gained resin:
Solids content: 46-49%
PH value: 7.5-8.0
Viscosity (25 ℃): 130-190mPas
Curing speed: 100-130s
Free formaldehyde content: 0.02%
Storage period:＞30 days
[comparative example one]
The composition of raw materials of table 3 comparative example one
Annotate: F and U represent respectively the formaldehyde solution that adds and the weight number of urea, U
1-U
3Represent respectively the weight number of the urea of first to the 3rd batch of adding, f and u represent respectively the mole number of formaldehyde and urea, u
1-u
3The mole number that represents respectively the urea of first to the 3rd batch of adding, f/u represent the mole number of formaldehyde and the ratio of the mole number of urea.
Concrete reactions steps is as follows:
1) 37% industrial formol is added reactor, transfer pH=8.8-9.0 with sodium hydroxide, add U
1, be warming up to 95 ℃ with 30-40 minute, be incubated 60 minutes;
2) transfer pH=4.2-4.8 with formic acid, add trimeric cyanamide, react to viscosity: 120-150mPas(30 ℃);
3) transfer pH to 6.0-6.5 with sodium hydroxide, add U
2, react to viscosity: 180-200mPas(30 ℃);
4) transfer pH=7.0-7.5 with sodium hydroxide, be cooled to 70 ℃, add U
3, insulation reaction 20 minutes;
5) be cooled to 40 ℃ with bottom discharge.
The resin quality index:
Solids content: 50-52%
PH value: 7.5-8.0
Viscosity (25 ℃): 160-200mPas
Curing speed: 90-120s
Free formaldehyde content: 0.2%
Storage period:＞30 days
[comparative example two]
The composition of raw materials of table 4 comparative example two
Annotate: F and U represent respectively the formaldehyde solution that adds and the weight number of urea, U
1-U
5Represent respectively the weight number of the urea of first to the 5th batch of adding, f and u represent respectively the mole number of formaldehyde and urea, u
1-u
5The mole number that represents respectively the urea of first to the 5th batch of adding, f/u represent the mole number of formaldehyde and the ratio of the mole number of urea.
Concrete reactions steps is as follows:
1) 37% formaldehyde solution is once added in the reactor, open steam heating to 30-40 ℃, steam off;
2) transfer pH=8.8 with sodium hydroxide, add U
1, steam off when then opening steam valve and being warmed up to 60-70 ℃ allows it from being warming up to 90 ℃, insulation reaction 60 minutes;
3) transfer pH to 6.5 with sodium hydroxide, add U
2, reacted 40 minutes;
4) transfer pH to 5.8 with formic acid, add U
3, add simultaneously trimeric cyanamide, 90 ℃ of lower reactions 20 minutes;
5) transfer pH to 4.8 with formic acid, react to viscosity: be coated with-4 glasss 23-25s(30 ℃);
6) transfer pH to 6.0 with sodium hydroxide, add U
4, react to viscosity: be coated with-4 glasss 30-33s(30 ℃);
7) transfer pH to 7.2 with sodium hydroxide, be cooled to 65 ℃, add U
5, insulation reaction 20 minutes;
8) be cooled to 40 ℃ with downward modulation pH=8.0, discharging.
The quality index of gained resin:
Solids content: 52-54%
PH value: 7.5-8.0
Viscosity (25 ℃): 110-150mPas
Curing speed: 100-130s
Free formaldehyde content: 0.1%
Storage period:＞30 days
[test example one]
The natural plant modification that utilizes the embodiment of the invention one, embodiment two methods to obtain is protected urea-formaldehyde resin adhesive that urea-formaldehyde resin adhesive and comparative example one, comparative example two methods obtain and is utilized continuous flat press to produce 8mm and 5mm produces medium density fibre board (MDF), produce when stablizing 1h and take a sample, wherein, test specimen 1 and test specimen 3 are the planks with embodiment one, the compacting of embodiment two patent formulation resins; Test specimen 2 and test specimen 4 are planks of comparative example one, comparative example two common urea-formaldehyde resin compactings.
According to prescriptive procedure among the GB/T 11718-2009 " medium density fibre board (MDF) " test specimen 1,2,3 and 4 is detected.It is as shown in the table for mean value as a result:
Table 5
Annotate: the physical and chemical index of sheet material is pressed GB/T 11718-2009 medium density fibre board (MDF) standard detection.
By as seen from Table 5, utilize natural plant modified urea-formaldehyde resin of the present invention to make medium density fibre board (MDF), with the fiberboard contrast of common modified urea-formaldehyde resin compacting, test specimen 1 and 3 mechanical performance index be a little less than test specimen 2 and 4, but all be higher than the requirement of indoor moisture proof based plate; Test specimen 1 and 3 burst size of methanal be a little more than test specimen 2 and 4, but all far below F****, E
0, the formaldehyde that requires of CARB Ш stage discharges, and test specimen 2 can only reach E reluctantly
0, the formaldehyde that requires of CARB Ш stage discharges, test specimen 4 can only reach GB E1 standard.
Carry out cost analysis as an example of the 8mm fiberboard example, the glue cost that adopts every cubic metre of natural plant modified urea-formaldehyde resin of the present invention is 1.78*190=338.2 unit, adopting every cube of rice glue cost of common urea-formaldehyde resin is 2.05*180=369 unit, and every cubic metre with saving 30.8 yuan on the glue unit consumption;
Carry out cost analysis as an example of the 5mm fiberboard example, the glue cost that adopts every cubic metre of natural plant modified urea-formaldehyde resin of the present invention is 1.41*200=282 unit, adopting every cube of rice glue cost of common urea-formaldehyde resin is 1.8*190=342 unit, and every cubic metre with saving 60 yuan on the glue unit consumption.
Analysis-by-synthesis adopts the fiberboard of natural plant modified urea-formaldehyde resin production of the present invention as can be known, and its physicochemical property surmounts the requirement of GB moist-proof board far away, and burst size of methanal can reach Europe superscript E
0, Japanese F****, U.S. CARB Ш stage requirement, be used for interior decoration, Furniture manufacture, automotive trim, packaging industry and all can satisfy export requirement.Every cubic metre with saving 30-60 unit on the glue unit consumption.
Claims (9)
1. the preparation method of a natural plant modified urea-formaldehyde resin is characterized in that, is comprised of the synthesis step of vegetable jelly resin and the synthesis step of vegetable jelly modified urea-formaldehyde resin; Wherein the raw material of the synthesis step of vegetable jelly resin is by weight percentage: water 85-91%, vegetable jelly 2.5-8%, trolamine 0.1-0.2%, the glyoxal solution 1.5-4% of mass concentration 39.5-40.5%, anhydrous sodium carbonate 0.1-0.5%, urea 1-3%, the formaldehyde solution 2-6% of mass concentration 36.5-37.4%, the ammoniacal liquor 1-4% of mass concentration 25%, trimeric cyanamide 0.2-1%;
1) the synthetic concrete steps of vegetable jelly resin are as follows:
A, slowly add vegetable jelly in the water, and stir;
B, vegetable jelly dissolve rear adding trolamine fully, survey pH=8.5-9.0, are warming up to 55-60 ℃ of insulation, reach 800-1200mPas(25 ℃ to viscosity);
C, reach add after the viscosity pH adjusting agent to pH be 5.0-6.0, add glyoxal solution, then add the urea of anhydrous sodium carbonate and 0.5-1.5%, insulation 1-2h;
D, adding formaldehyde solution, ammoniacal liquor and trimeric cyanamide;
E, be warming up to 80-85 ℃, be incubated to viscosity reach 1000-1600mPas(25 ℃), then begin cooling;
F, when being cooled to 40-45 ℃, add pH adjusting agent to pH=7.0-7.5, add the urea of 0.5-2.5%, insulation 20-30min, rear discharging stirs;
The raw material of vegetable jelly modified urea-formaldehyde resin synthesis step is by weight percentage: the vegetable jelly resin 45-60% that step 1) is synthetic, the formaldehyde solution 20-38% of mass concentration 36.5-37.4%, urotropine 0.1-0.3%, urea 15-30%, trimeric cyanamide 0.5-2%; The concrete steps that the vegetable jelly modified urea-formaldehyde resin synthesizes are as follows:
G, formaldehyde solution, urotropine mixed transfer pH to 7.0-7.5, add first urea, wherein formaldehyde is 2.0-3.0:1 with the ratio of the mole number of first urea;
H, be warmed up to 85-95 ℃, insulation 30-50min;
I, adding pH adjusting agent continue reaction 80-100min to pH to 4.5-5.5;
J, add pH adjusting agent to pH to 5.2-5.6, add second batch urea, the mole number that makes the formaldehyde that adds among the step G is 1.5-1.9:1 with the ratio of the total mole number of two batches of urea, continues to react to viscosity 100-300mPas(25 ℃);
K, add pH adjusting agent and transfer pH to 7.0-7.5, add the urea of surplus, the mole number that makes the formaldehyde that adds among the step G is 0.8-1.4:1 with the ratio of the total mole number of three batches of urea, begins cooling;
L, be cooled to 65-75 ℃, add trimeric cyanamide, insulation 10-20min;
M, the synthetic vegetable jelly resin of adding step 1) stir 15-30min, are cooled to 35-40 ℃, add pH adjusting agent to pH to 7.5-8.5 discharging and namely get the vegetable jelly modified urea-formaldehyde resin.
2. the preparation method of natural plant modified urea-formaldehyde resin according to claim 1 is characterized in that, described vegetable jelly is one or more in sesbania gum, guar gum, xanthan gum, the Viscogum BE.
3. the preparation method of natural plant modified urea-formaldehyde resin according to claim 1 is characterized in that, the pH adjusting agent among described step F, J, K, the M is one or more in ammoniacal liquor, sodium hydroxide solution or the trolamine.
4. the preparation method of natural plant modified urea-formaldehyde resin according to claim 1 is characterized in that, the pH adjusting agent among described step C, the I is selected from one or more in formic acid, oxalic acid, citric acid, the tartrate.
5. the preparation method of natural plant modified urea-formaldehyde resin according to claim 1 is characterized in that, the formaldehyde that adds among the described step G is 2.24:1 with the ratio of the mole number of first urea, and it is 50 ℃ that urea adds temperature.
6. the preparation method of natural plant modified urea-formaldehyde resin according to claim 1 is characterized in that, under the described step J condition, the reaction times is 80-100min, and reaction solution viscosity should be controlled 150-250mPas(25 ℃).
7. the preparation method of natural plant modified urea-formaldehyde resin according to claim 1 or 5 is characterized in that, among the described step J, the formaldehyde that adds among the step G is 1.78:1 with the ratio of the total mole number of two batches of urea, and it is 90 ℃ that urea adds temperature.
8. the preparation method of natural plant modified urea-formaldehyde resin according to claim 1 is characterized in that, in the described step K, the formaldehyde that adds among the step G is 0.82:1 with the ratio of the total mole number of three batches of urea, and it is 85 ℃ that urea adds temperature.
9. the preparation method of natural plant modified urea-formaldehyde resin according to claim 7 is characterized in that, in the described step K, the formaldehyde that adds among the step G is 0.82:1 with the ratio of the total mole number of three batches of urea, and it is 85 ℃ that urea adds temperature.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104559871A (en) * | 2013-10-22 | 2015-04-29 | 寿光市东宇鸿翔木业有限公司 | Urea-formaldehyde glue curing agent and preparation method thereof |
| CN104559872A (en) * | 2013-10-22 | 2015-04-29 | 寿光市东宇鸿翔木业有限公司 | Urea-formaldehyde glue for furniture-paper impregnation and preparation method of urea-formaldehyde glue |
| CN104559863A (en) * | 2013-10-22 | 2015-04-29 | 寿光市东宇鸿翔木业有限公司 | Urea-formaldehyde glue and preparation method thereof |
| CN111331703A (en) * | 2020-04-07 | 2020-06-26 | 香河众旺木业有限公司 | Medium-density board 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 |
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Patent Citations (1)
| 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104559871A (en) * | 2013-10-22 | 2015-04-29 | 寿光市东宇鸿翔木业有限公司 | Urea-formaldehyde glue curing agent and preparation method thereof |
| CN104559872A (en) * | 2013-10-22 | 2015-04-29 | 寿光市东宇鸿翔木业有限公司 | Urea-formaldehyde glue for furniture-paper impregnation and preparation method of urea-formaldehyde glue |
| CN104559863A (en) * | 2013-10-22 | 2015-04-29 | 寿光市东宇鸿翔木业有限公司 | Urea-formaldehyde glue and preparation method thereof |
| CN111331703A (en) * | 2020-04-07 | 2020-06-26 | 香河众旺木业有限公司 | Medium-density board and preparation method thereof |
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| CN103319674B (en) | 2015-03-04 |
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