CN106632936A - Preparation method for water-resistant anti-aging modified urea resin - Google Patents
Preparation method for water-resistant anti-aging modified urea resin Download PDFInfo
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Abstract
The invention relates to a preparation method for water-resistant anti-aging modified urea resin, and belongs to the technical field of urea resin preparation. According to the preparation method, fat particles in soybean milk float because of cooling to obtain bean fat oil leather; grease is decomposed in a fermenting liquid under the action of microbes; the number of hydrophobic resin groups in a urea formaldehyde resin matrix is increased, so that the water resistance of the resin is improved; montmorillonoid is coated by using peach gum first by utilizing an ultraviolet ray shielding function of the montmorillonoid, so that the interfacial compatibility of the montmorillonoid and the resin matrix is increased; the montmorillonoid is doped into the resin under the action of a coupling agent, and finally, the modified urea resin is obtained, so that the anti-aging performance of the modified urea resin is obviously improved. The water-resistant anti-aging modified urea resin prepared by the invention has extremely good water resistance and anti-aging performance, and has a broad application prospect.
Description
Technical field
The present invention relates to a kind of preparation method of water-fast anti-aging modified urea-formaldehyde resin, belongs to Lauxite technology of preparing neck
Domain.
Background technology
Lauxite, also known as urea formaldehyde resin, is urea with formaldehyde under catalyst, alkalescence or acidic catalyst effect, contracting
Initial stage Lauxite is polymerized to, then again under curing agent or promoter effect, insoluble, insoluble latter stage thermosetting resin is formed.Gu
Lauxite color after change is more shallow than phenolic resin, and be translucent shape, and weak acid resistant, weak base, good insulation preformance, wearability is splendid,
Low price, it is the maximum kind of consumption in adhesive, particularly in the manufacture of the various wood-based plates of wood-processing industry, ureaformaldehyde
Resin and its modified product account for 90% or so of the total consumption of adhesive.Easily decompose however, existing and meeting strong acid, highly basic, weatherability compared with
Difference, just viscous poor, contraction is big, fragility is big, not water-fast, easily aging problem, although Lauxite also can be consolidated under heating or at room temperature
Change, but hardening time is long, and solidification is incomplete, it is necessary to which it is modified, and improves performance, expands application.
Lauxite is the main binder of domestic and international timber industry, due to its bonding strength height, quick solidifying, operability
Good, low production cost, abundant raw material the series of advantages such as are easy to get and are used widely.But the weatherability of Lauxite compared with
Difference, not water-fast, easily aging problem significantly limit its application in every respect.Therefore, invent a kind of water-fast anti-aging
Modified urea-formaldehyde resin can greatly widen the range of application of Lauxite, with splendid Research Prospects.
The content of the invention
Present invention mainly solves technical problem, there is weatherability for current Lauxite poor, not water-fast, easily aging
Defect, there is provided one kind boils hot soya-bean milk, and the outermost layer of skin is extracted in cooling, by montmorillonite and peach gum blending cladding, in butter fruit and peanut
By the outermost layer of skin, montmorillonite and Lauxite coupling reaction in the presence of zymotic fluid, the side of water-fast anti-aging Lauxite is finally obtained
Method.The present invention obtains beans fatty oil skin using the floating of catching a cold of the lipochondrion in soya-bean milk, makes in the presence of microorganism in zymotic fluid
Grease decomposes, and increases the hydrophobicity ester group quantity in Lauxite matrix, improves the resistance to water of resin, recycles and covers de-
The function of shielding ultraviolet radiation of soil, is coated first with peach gum to it, increases the interface compatibility of montmorillonite and resin matrix, is being coupled
It is doped in the presence of agent in resin, final modified urea-formaldehyde resin so as to which ageing resistace is significantly improved.It is of the invention obtained
Water-fast anti-aging Lauxite has splendid resistance to water and ageing resistace, has broad application prospects.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）The soybean shieve dust impurity of full grains is chosen, is put in peeling machine and is crushed peeling, blown crust with hair-dryer
Only, the soya bean of peeling is put in wooden barrel, adds water up to soya bean and be submerged by water completely, 7～9h is standing and soak for, by the Huang after immersion
Beans and water are 1 in mass ratio:Stone mill defibrination is poured into after 10 mixing, collect juice；
（2）The juice of above-mentioned collection is filtered and removes filter residue, obtain filtrate, as soya-bean milk, the heating soybean milk for obtaining is boiled, treated
Soya-bean milk after boiling is poured in ceramic pot after being cooled to 70～80 DEG C, hot soya-bean milk cooling after 10～15min is stood, in soya-bean milk
Lipochondrion float, form the fine and close outermost layer of skin, press from both sides out the outermost layer of skin with tweezers, it is standby；
（3）Weigh montmorillonite and be put in nano-level grinder 500 mesh sieves excessively after 2～3h of grinding, obtain montmorillonite powder, gained is covered
De- soil powder and peach gum are 2 in mass ratio:After 1 mixing, the deionized water of 8～10 times of both gross masses, heat temperature raising are added
Mixed liquor is obtained to 70～80 DEG C of stirring 20～30min of mixing, then mixed liquor is moved in cucurbit, continue to be heated to 95～
100 DEG C, moisture removal is removed in distillation, obtains the montmorillonite powder of peach gum cladding, standby；
（4）Take etc. quality butter fruit and peanut be put into crush in tissue pulverizer after be placed in ceramic pot, add water in tank straight
To both crushed materials are totally submerged, the bottom liquid that ferments, then the newborn microbacterium that its gross mass 0.2% is added in fermentation bottom liquid are obtained
Bacterial classification, heat-preservation fermentation 10～12 days at 30～40 DEG C, is separated by filtration after fermentation ends and obtains filtrate, be i.e. mixed fermentation liquid；
（5）In mass ratio it is 50:1 by Lauxite and step（3）Load anti-after the montmorillonite powder mixing of standby peach gum cladding
In answering kettle, then the above-mentioned mixed fermentation liquid of Lauxite quality 5% is added in reactor, at 60～70 DEG C stirring mixing 1～
2h, obtains pre-processing resin；
（6）By above-mentioned pretreatment resin and step（2）The standby outermost layer of skin and trypsase is 500 in mass ratio:10:1 mixing
It is fitted into afterwards in ceramic pot, reactant is moved into into reactor after 6～8h of insulation reaction at 30～40 DEG C, then adds in reactor
The Silane coupling agent KH550 of reactant gross mass 1～3%, is warming up to 40～50 DEG C of continuation 2～3h of stirring reaction, after reaction terminates
Discharge and move into drying in vacuum drying chamber and remove moisture removal, obtain final product water-fast anti-aging Lauxite.
The application process of the present invention：Count by weight, by water-fast anti-aging ureaformaldehyde tree obtained in 10～15 parts of present invention
Do after fat, 30～40 parts of wood powders, 20～30 parts of paper pulp, 0.5～0.8 part of curing agent, 3～5 parts of lubricants, 3～5 parts of thiocarbamide mixing
Dry crushing, obtains urea-formaldehyde moulding powder, and moudling powder is poured in stainless steel mould, with the pressure of 25～35MPa at 140～150 DEG C
Form removal after power 10～15min of hot pressing obtains final product urea-formaldehyde plastics product, and after testing plastic products obtained in Lauxite of the present invention are used
Life-span extends 2～3 years than traditional Lauxite plastic products, and ageing resistance is splendid, is obtained with Lauxite of the present invention bonding
Test specimen in 90～100 DEG C of thermostat water bath after 10～12h of boiling, bonding strength up to 1.6～1.8MPa, with excellent
Resistance to water, application is wide.
The invention has the beneficial effects as follows：
（1）Obtained water-fast anti-aging Lauxite preparing raw material of the invention is easy to get, and preparation process is simple to operation, low cost
It is honest and clean；
（2）Obtained water-fast anti-aging Lauxite of the invention has splendid resistance to water, is made with Lauxite of the present invention bonding
In 80～100 DEG C of thermostat water bath after 8～10h of boiling, bonding strength is up to 1.7～2.0MPa for the test specimen for obtaining；
（3）Plastic products service life obtained in Lauxite of the present invention extends 2～3 than traditional Lauxite plastic products
Year, ageing resistance is splendid.
Specific embodiment
The soybean shieve dust impurity of full grains is chosen, is put in peeling machine and is crushed peeling, blown crust with hair-dryer
Only, the soya bean of peeling is put in wooden barrel, adds water up to soya bean and be submerged by water completely, 7～9h is standing and soak for, by the Huang after immersion
Beans and water are 1 in mass ratio:Stone mill defibrination is poured into after 10 mixing, collect juice；The juice of above-mentioned collection is filtered and removes filter residue,
Filtrate, as soya-bean milk are obtained, the heating soybean milk for obtaining is boiled, the soya-bean milk after boiling is poured after being cooled to 70～80 DEG C
In ceramic pot, hot soya-bean milk cooling after 10～15min is stood, the lipochondrion in soya-bean milk floats, form the fine and close outermost layer of skin, pressed from both sides with tweezers
Go out the outermost layer of skin, it is standby；Weigh montmorillonite and be put in nano-level grinder 500 mesh sieves excessively after 2～3h of grinding, obtain montmorillonite powder, will
Gained montmorillonite powder and peach gum are 2 in mass ratio:After 1 mixing, the deionized water of 8～10 times of both gross masses is added, plus
Heat is warming up to 70～80 DEG C of stirring 20～30min of mixing and obtains mixed liquor, then mixed liquor is moved in cucurbit, continues to be heated to
95～100 DEG C, moisture removal is removed in distillation, obtains the montmorillonite powder of peach gum cladding, standby；The butter fruit and peanut for the quality such as taking is put
Enter and be placed in ceramic pot after crushing in tissue pulverizer, add water in tank up to both crushed materials are totally submerged, fermented
Bottom liquid, then the newborn microbacterium bacterial classification of its gross mass 0.2%, the heat-preservation fermentation 10～12 at 30～40 DEG C are added in fermentation bottom liquid
My god, it is separated by filtration after fermentation ends and obtains filtrate, be i.e. mixed fermentation liquid；In mass ratio it is 50:1 by Lauxite and standby peach gum
It is fitted in reactor after the montmorillonite powder mixing of cladding, then adds the above-mentioned mixing of Lauxite quality 5% to send out in reactor
Zymotic fluid, 1～2h of stirring mixing at 60～70 DEG C, obtains pre-processing resin；By above-mentioned pretreatment resin and the standby outermost layer of skin with
And trypsase is 500 in mass ratio:10:It is fitted in ceramic pot after 1 mixing, will after 6～8h of insulation reaction at 30～40 DEG C
Reactant moves into reactor, then the Silane coupling agent KH550 of reactant gross mass 1～3% is added in reactor, is warming up to 40
～50 DEG C of continuation 2～3h of stirring reaction, reaction discharges after terminating and moves into drying in vacuum drying chamber and removes moisture removal, obtains final product water-fast
Anti-aging Lauxite.
Example 1
The soybean shieve dust impurity of full grains is chosen, is put in peeling machine and is crushed peeling, blown off crust with hair-dryer, will
The soya bean of peeling is put in wooden barrel, is added water up to soya bean and is submerged by water completely, is standing and soak for 7h, and the soya bean after immersion and water are pressed
Mass ratio is 1:Stone mill defibrination is poured into after 10 mixing, collect juice；The juice of above-mentioned collection is filtered and removes filter residue, filtered
Liquid, as soya-bean milk, the heating soybean milk for obtaining is boiled, and the soya-bean milk after boiling is poured in ceramic pot after being cooled to 70 DEG C,
Hot soya-bean milk cooling after 10min is stood, the lipochondrion in soya-bean milk floats, form the fine and close outermost layer of skin, with tweezers the outermost layer of skin is pressed from both sides out, it is standby；
Weigh montmorillonite and be put in nano-level grinder to grind and cross after 2h 500 mesh sieves, obtain montmorillonite powder, by gained montmorillonite powder and
Peach gum is 2 in mass ratio:After 1 mixing, the deionized water of 8 times of both gross masses is added, be heated to 70 DEG C of stirring mixing
20min obtains mixed liquor, then mixed liquor is moved in cucurbit, continues to be heated to 95 DEG C, and moisture removal is removed in distillation, obtains peach gum bag
The montmorillonite powder for covering, it is standby；Take etc. quality butter fruit and peanut be put into crush in tissue pulverizer after be placed in ceramic pot,
Add water in tank up to both crushed materials are totally submerged, obtain the bottom liquid that ferments, then its gross mass is added in fermentation bottom liquid
0.2% newborn microbacterium bacterial classification, heat-preservation fermentation 10 days at 30 DEG C are separated by filtration after fermentation ends and obtain filtrate, be i.e. mixed fermentation
Liquid；In mass ratio it is 50:It is fitted in reactor after the 1 montmorillonite powder mixing for coating Lauxite and standby peach gum, then to
The above-mentioned mixed fermentation liquid of Lauxite quality 5% is added in reactor, the stirring mixing 1h at 60 DEG C obtains pre-processing resin；
In mass ratio it is 500 by above-mentioned pretreatment resin and the standby outermost layer of skin and trypsase:10:It is fitted in ceramic pot after 1 mixing,
Reactant is moved into into reactor after insulation reaction 6h at 30 DEG C, then the silane idol of reactant gross mass 1% is added in reactor
Connection agent KH550, is warming up to 40 DEG C of continuation stirring reactions 2h, and reaction discharges after terminating and moves into drying in vacuum drying chamber and goes eliminating water
Point, obtain final product water-fast anti-aging Lauxite.
Count by weight, by water-fast anti-aging Lauxite obtained in 10 parts of present invention, 30 parts of wood powders, 20 parts of paper pulp,
Drying and crushing after 0.5 part of curing agent, 3 parts of lubricants, 3 parts of thiocarbamide mixing, obtains urea-formaldehyde moulding powder, pours moudling powder into stainless steel
In mould, urea-formaldehyde plastics product is obtained final product with form removal after the pressure hot pressing 10min of 25MPa at 140 DEG C, after testing ureaformaldehyde of the present invention
Plastic products service life obtained in resin is extended 2 years than traditional Lauxite plastic products, and ageing resistance is splendid, with this
In 90 DEG C of thermostat water bath after boiling 10h, bonding strength has test specimen obtained in bright Lauxite bonding up to 1.6MPa
Excellent resistance to water, application is wide.
Example 2
The soybean shieve dust impurity of full grains is chosen, is put in peeling machine and is crushed peeling, blown off crust with hair-dryer, will
The soya bean of peeling is put in wooden barrel, is added water up to soya bean and is submerged by water completely, is standing and soak for 8h, and the soya bean after immersion and water are pressed
Mass ratio is 1:Stone mill defibrination is poured into after 10 mixing, collect juice；The juice of above-mentioned collection is filtered and removes filter residue, filtered
Liquid, as soya-bean milk, the heating soybean milk for obtaining is boiled, and the soya-bean milk after boiling is poured in ceramic pot after being cooled to 75 DEG C,
Hot soya-bean milk cooling after 13min is stood, the lipochondrion in soya-bean milk floats, form the fine and close outermost layer of skin, with tweezers the outermost layer of skin is pressed from both sides out, it is standby；
Weigh montmorillonite and be put in nano-level grinder to grind and cross after 2h 500 mesh sieves, obtain montmorillonite powder, by gained montmorillonite powder and
Peach gum is 2 in mass ratio:After 1 mixing, the deionized water of 9 times of both gross masses is added, be heated to 75 DEG C of stirring mixing
25min obtains mixed liquor, then mixed liquor is moved in cucurbit, continues to be heated to 98 DEG C, and moisture removal is removed in distillation, obtains peach gum bag
The montmorillonite powder for covering, it is standby；Take etc. quality butter fruit and peanut be put into crush in tissue pulverizer after be placed in ceramic pot,
Add water in tank up to both crushed materials are totally submerged, obtain the bottom liquid that ferments, then its gross mass is added in fermentation bottom liquid
0.2% newborn microbacterium bacterial classification, heat-preservation fermentation 11 days at 35 DEG C are separated by filtration after fermentation ends and obtain filtrate, be i.e. mixed fermentation
Liquid；In mass ratio it is 50:It is fitted in reactor after the 1 montmorillonite powder mixing for coating Lauxite and standby peach gum, then to
The above-mentioned mixed fermentation liquid of Lauxite quality 5% is added in reactor, the stirring mixing 1h at 65 DEG C obtains pre-processing resin；
In mass ratio it is 500 by above-mentioned pretreatment resin and the standby outermost layer of skin and trypsase:10:It is fitted in ceramic pot after 1 mixing,
Reactant is moved into into reactor after insulation reaction 7h at 35 DEG C, then the silane idol of reactant gross mass 2% is added in reactor
Connection agent KH550, is warming up to 45 DEG C of continuation stirring reactions 2h, and reaction discharges after terminating and moves into drying in vacuum drying chamber and goes eliminating water
Point, obtain final product water-fast anti-aging Lauxite.
Count by weight, by water-fast anti-aging Lauxite obtained in 13 parts of present invention, 35 parts of wood powders, 25 parts of paper pulp,
Drying and crushing after 0.7 part of curing agent, 4 parts of lubricants, 4 parts of thiocarbamide mixing, obtains urea-formaldehyde moulding powder, pours moudling powder into stainless steel
In mould, urea-formaldehyde plastics product is obtained final product with form removal after the pressure hot pressing 13min of 30MPa at 145 DEG C, after testing ureaformaldehyde of the present invention
Plastic products service life obtained in resin is extended 2 years than traditional Lauxite plastic products, and ageing resistance is splendid, with this
Test specimen is in 95 DEG C of thermostat water bath after boiling 11h obtained in bright Lauxite bonding, and bonding strength is glued up to 1.7MPa
, up to 1.8MPa, with excellent resistance to water, application is wide for intensity.
Example 3
The soybean shieve dust impurity of full grains is chosen, is put in peeling machine and is crushed peeling, blown off crust with hair-dryer, will
The soya bean of peeling is put in wooden barrel, is added water up to soya bean and is submerged by water completely, is standing and soak for 9h, and the soya bean after immersion and water are pressed
Mass ratio is 1:Stone mill defibrination is poured into after 10 mixing, collect juice；The juice of above-mentioned collection is filtered and removes filter residue, filtered
Liquid, as soya-bean milk, the heating soybean milk for obtaining is boiled, and the soya-bean milk after boiling is poured in ceramic pot after being cooled to 80 DEG C,
Hot soya-bean milk cooling after 15min is stood, the lipochondrion in soya-bean milk floats, form the fine and close outermost layer of skin, with tweezers the outermost layer of skin is pressed from both sides out, it is standby；
Weigh montmorillonite and be put in nano-level grinder to grind and cross after 3h 500 mesh sieves, obtain montmorillonite powder, by gained montmorillonite powder and
Peach gum is 2 in mass ratio:After 1 mixing, the deionized water of 10 times of both gross masses is added, be heated to 80 DEG C of stirring mixing
30min obtains mixed liquor, then mixed liquor is moved in cucurbit, continues to be heated to 100 DEG C, and moisture removal is removed in distillation, obtains peach gum
The montmorillonite powder of cladding, it is standby；Take etc. quality butter fruit and peanut be put into crush in tissue pulverizer after be placed in ceramic pot
In, add water in tank up to both crushed materials are totally submerged, the bottom liquid that ferments is obtained, then add its gross mass in fermentation bottom liquid
0.2% newborn microbacterium bacterial classification, heat-preservation fermentation 12 days at 40 DEG C are separated by filtration after fermentation ends and obtain filtrate, be i.e. mixed fermentation
Liquid；In mass ratio it is 50:It is fitted in reactor after the 1 montmorillonite powder mixing for coating Lauxite and standby peach gum, then to
The above-mentioned mixed fermentation liquid of Lauxite quality 5% is added in reactor, the stirring mixing 2h at 70 DEG C obtains pre-processing resin；
In mass ratio it is 500 by above-mentioned pretreatment resin and the standby outermost layer of skin and trypsase:10:It is fitted in ceramic pot after 1 mixing,
Reactant is moved into into reactor after insulation reaction 8h at 40 DEG C, then the silane idol of reactant gross mass 3% is added in reactor
Connection agent KH550, is warming up to 50 DEG C of continuation stirring reactions 3h, and reaction discharges after terminating and moves into drying in vacuum drying chamber and goes eliminating water
Point, obtain final product water-fast anti-aging Lauxite.
Count by weight, by water-fast anti-aging Lauxite obtained in 15 parts of present invention, 40 parts of wood powders, 30 parts of paper pulp,
Drying and crushing after 0.8 part of curing agent, 5 parts of lubricants, 5 parts of thiocarbamide mixing, obtains urea-formaldehyde moulding powder, pours moudling powder into stainless steel
In mould, urea-formaldehyde plastics product is obtained final product with form removal after the pressure hot pressing 15min of 35MPa at 150 DEG C, after testing ureaformaldehyde of the present invention
Plastic products service life obtained in resin is extended 3 years than traditional Lauxite plastic products, and ageing resistance is splendid, with this
In 100 DEG C of thermostat water bath after boiling 12h, bonding strength is up to 1.8MPa, tool for test specimen obtained in bright Lauxite bonding
There is excellent resistance to water, application is wide.
Claims (1)
1. a kind of preparation method of water-fast anti-aging modified urea-formaldehyde resin, it is characterised in that concrete modification procedure is：
（1）The soybean shieve dust impurity of full grains is chosen, is put in peeling machine and is crushed peeling, blown crust with hair-dryer
Only, the soya bean of peeling is put in wooden barrel, adds water up to soya bean and be submerged by water completely, 7～9h is standing and soak for, by the Huang after immersion
Beans and water are 1 in mass ratio:Stone mill defibrination is poured into after 10 mixing, collect juice；
（2）The juice of above-mentioned collection is filtered and removes filter residue, obtain filtrate, as soya-bean milk, the heating soybean milk for obtaining is boiled, treated
Soya-bean milk after boiling is poured in ceramic pot after being cooled to 70～80 DEG C, hot soya-bean milk cooling after 10～15min is stood, in soya-bean milk
Lipochondrion float, form the fine and close outermost layer of skin, press from both sides out the outermost layer of skin with tweezers, it is standby；
（3）Weigh montmorillonite and be put in nano-level grinder 500 mesh sieves excessively after 2～3h of grinding, obtain montmorillonite powder, gained is covered
De- soil powder and peach gum are 2 in mass ratio:After 1 mixing, the deionized water of 8～10 times of both gross masses, heat temperature raising are added
Mixed liquor is obtained to 70～80 DEG C of stirring 20～30min of mixing, then mixed liquor is moved in cucurbit, continue to be heated to 95～
100 DEG C, moisture removal is removed in distillation, obtains the montmorillonite powder of peach gum cladding, standby；
（4）Take etc. quality butter fruit and peanut be put into crush in tissue pulverizer after be placed in ceramic pot, add water in tank straight
To both crushed materials are totally submerged, the bottom liquid that ferments, then the newborn microbacterium that its gross mass 0.2% is added in fermentation bottom liquid are obtained
Bacterial classification, heat-preservation fermentation 10～12 days at 30～40 DEG C, is separated by filtration after fermentation ends and obtains filtrate, be i.e. mixed fermentation liquid；
（5）In mass ratio it is 50:1 by Lauxite and step（3）Load anti-after the montmorillonite powder mixing of standby peach gum cladding
In answering kettle, then the above-mentioned mixed fermentation liquid of Lauxite quality 5% is added in reactor, at 60～70 DEG C stirring mixing 1～
2h, obtains pre-processing resin；
（6）By above-mentioned pretreatment resin and step（2）The standby outermost layer of skin and trypsase is 500 in mass ratio:10:1 mixing
It is fitted into afterwards in ceramic pot, reactant is moved into into reactor after 6～8h of insulation reaction at 30～40 DEG C, then adds in reactor
The Silane coupling agent KH550 of reactant gross mass 1～3%, is warming up to 40～50 DEG C of continuation 2～3h of stirring reaction, after reaction terminates
Discharge and move into drying in vacuum drying chamber and remove moisture removal, obtain final product water-fast anti-aging Lauxite.
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