CN104910842B - Preparation method of resorcinol modified urea-formaldehyde resin adhesive - Google Patents
Preparation method of resorcinol modified urea-formaldehyde resin adhesive Download PDFInfo
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- CN104910842B CN104910842B CN201510390618.8A CN201510390618A CN104910842B CN 104910842 B CN104910842 B CN 104910842B CN 201510390618 A CN201510390618 A CN 201510390618A CN 104910842 B CN104910842 B CN 104910842B
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Abstract
The invention discloses a preparation method of resorcinol modified urea-formaldehyde resin adhesive. The method is that the weak acid to weak alkali to weak acid to weak alkali synthesizing process is adopted; resorcinol is added to be used as a modifying agent to prepare the urea-formaldehyde resin adhesive. The method is simple in process, simple and convenient to operate, and suitable for industrial production; the prepared urea-formaldehyde resin adhesive contains 0.05 to 0.06% of free formaldehyde; the formaldehyde emission of plywood prepared from the adhesive reaches E0 level stand; in addition, the cementing strength reaches II type plywood standard.
Description
Technical field
The invention belongs to organic binder bond technical field, and in particular to the preparation of resorcinol modified urea-formaldehyde resin adhesive
Method.
Background technology
With developing rapidly for science and technology, people increasingly pay attention to producing the coordinated development with environmental protection.For wood
For material processing industry, based Wood Adhesives can manufacture in process of production a large amount of pollutants, and urea-formaldehyde resin adhesive adds as timber
One of major product of industrial and commercial bank's industry, will be consumed in a large number in process every year.Lauxite (UF) is a kind of comprehensive
Energy preferably adhesive, such as adhesive strength is high, there is certain resistance to water, and fast, the excellent water solubility of curing rate, tack is good,
It is especially cheap, therefore enjoy the favor of wood-processing industry.However, there is free formaldehyde content height in UF, in hot setting
Excitant toxic gas is discharged during making sheet, the healthy of people in serious harm.With the continuous improvement of living standards of the people
With reinforcement of the consumers in general to social environment consciousness, urea-formaldehyde resin adhesive is put forward higher requirement, low content of free formaldehyde
The high performance urea-formaldehyde resin adhesive of content has become noticeable research topic.
China discloses pressure standard GB 18580-2001 in January, 2002《Indoor decorating and refurnishing materials wood-based plate and its system
Form aldehyde release limitation in product》, since enforcement, though the artificial board formaldehyde release problem of China is greatly taken on a new look, market sampling observation
Plywood product burst size of methanal also can only achieve E2 levels mostly, and E1 levels have exceeded phenomenon, E nor a lot0Level
Proportion very little very little (E0Level is the most stringent of environmental protection standard of requirement), and mostly rely on external import.To improve me
State's Lauxite industry domestic and international market competitiveness, it is necessary to which the ureaformaldehyde tree of low burst size of methanal is developed by technical research
Fat adhesive, and pay attention to timely conversion of the scientific and technological achievement to industrialization.
In recent years, using modifier modification urea-formaldehyde resin adhesive, existing some patent reports.Chinese invention patent
CN20151005588.5 discloses a kind of urea-formaldehyde resin adhesive and its preparation technology of ultra-low formaldehyde release, first uses hydroxide
Sodium adjusts the pH value of formalin, is subsequently adding urea reaction, controls pH value in reaction by the way that formic acid is added dropwise in the process, then
In the case of certain viscosity, pH value is adjusted with NaOH, add hydroxymethyl cellulose, add reacting aluminum sulfate, use first
Acid for adjusting pH value, adds polyvinyl alcohol and pure water reaction, is down to the urea-formaldehyde resin adhesive that room temperature is obtained ultra-low formaldehyde release
Stick.Chinese invention patent CN201410792505 discloses a kind of preparation method of low-poison urea-formaldehyde resin adhesive, including following step
Suddenly：Urea, Jing steam is added to heat up, obtain being not less than 6.7 urea and formalin in formalin；Again to the solution
Middle addition boric acid, then adds 5-15% formic acid every 5-8min, adds melamine, and at 88-91 DEG C polycondensation reaction is carried out, when
Viscosity adds triethanolamine up to after 17.5-18.5Pas, adjusts the pH to 6.5-6.9 of mixed reaction solution, obtains urea-formaldehyde resin adhesive；
To urea-formaldehyde resin adhesive, at 84-85 DEG C, urea is added, control pH for 6.3-6.6, insulation reaction 8-12min；It is cooled to 64-65 DEG C
Add urea again afterwards, when progressively cooling down is to less than 40 DEG C, adjust pH value to 8.0-8.3, terminating reaction, obtain low toxicity ureaformaldehyde
Resin glue.
Above-mentioned preparation method can be obtained the low urea-formaldehyde resin adhesive of burst size of methanal, but not have been reported that its formaldehyde is released
E can high-volume be reached0Level standard, it is therefore necessary to develop the new method of urea-formaldehyde resin adhesive preparation, to be obtained interior is met
The urea-formaldehyde resin adhesive that decoration is used, the present invention is therefore.
The content of the invention
For the deficiencies in the prior art, it is an object of the invention to provide a kind of resorcinol modified urea-formaldehyde resin adhesive
Preparation method, urea-formaldehyde resin adhesive free formaldehyde content obtained in the method is low, obtained glued board burst size of methanal is little.
In order to solve these problems of the prior art, the technical scheme that the present invention is provided is：
A kind of preparation method of resorcinol modified urea-formaldehyde resin adhesive, comprises the following steps：
(1) 37% formalin is added equipped with reactor, stirring is warming up to 45～55 DEG C, with 5～10%
It is 5.0～6.5 that NaOH solution adjusts pH, adds first urea, stirring to be warming up to 80～90 DEG C, 20～30min of insulation reaction；
(2) the NaOH solution regulation pH for adding 5～10% is 8.0～9.0, addition second batch urea, insulation reaction 20～
30min；
(3) resorcinol is added, is incubated after 10～15min and adds 15～20% NH4Cl solution adjust pH be 5.0～
5.5, add the 3rd batch of urea to continue to react, drawn in the hot water that glue instills 40 DEG C or so with glue head dropper is continual, when
Occur reacting 10～20min again after atomizating phenomenon；
(4) the NaOH solution regulation pH for adding 5～10% is 8.0～9.0, adds the 4th batch of urea, reacts 20～25min
15～20% NH is added afterwards4Cl solution adjusts pH to 7.5～8.0；
(5) when temperature is down to room temperature, filtering and discharging.
In preferred technical scheme, the mol ratio of formaldehyde and urea total amount is 1.1: 1.
In preferred technical scheme, first urea accounts for the 60～70% of urea total amount in the step (1), the step
(2) second batch urea accounts for the 10～15% of urea total amount in, in the step (3) the 3rd batch of urea account for urea total amount 10～
15%, the 4th batch of urea accounts for the 5～10% of urea total amount in the step (4).
In preferred technical scheme, resorcinol accounts for the 4～5% of urea total amount in the step (3).
Relative to scheme of the prior art, it is an advantage of the invention that：
1st, technical scheme is adopted, using weak acid-weak base-weak acid-weak base synthesis technique, and resorcinol is added
As modifying agent to prepare urea-formaldehyde resin adhesive, process is simple, and convenient operation, obtained urea-formaldehyde resin adhesive dissociates
Content of formaldehyde is low；
2nd, technical scheme is adopted, the glued board formaldehyde made using urea-formaldehyde resin adhesive obtained in the method
Burst size can reach E0Level standard, and the resistance to water of glued board is more preferably, and its intensity reaches II class glued board standards.
Specific embodiment
Such scheme is described further below in conjunction with specific embodiment.It should be understood that these embodiments are for illustrating
The present invention and be not limited to limit the scope of the present invention.The implementation condition adopted in embodiment can be done according to the condition of concrete producer
Further adjustment, not marked implementation condition is usually the condition in normal experiment.
First, urea-formaldehyde resin adhesive fluidity matter is determined：Use Na2SO3Method determines the free first of above-mentioned prepared Lauxite glue
Aldehyde；With -4 glasss of viscosimeters are applied, according to national standard《The dope viscosity determination methods of GB/T 1723》The method of testing of regulation is determined
The viscosity of above-mentioned prepared Lauxite glue；According to national standard《GB/T 14074-2006》The method of testing of regulation is surveyed
Hardening time, the solid content of fixed above-mentioned prepared Lauxite glue.
2nd, the making and performance test of glued board
1st, the making of three layers of glued board
(1) glue：According to m (UF): m (ammonium chloride)=100: 1 ratio, above-mentioned material is well mixed；
(2) linden veneer：Breadth is 300mm × 300mm × 1mm, and moisture content is 8%-12%, and double spread amount is
230g/m2-250g/m2, then by the parallel rift grain of two panels examination material to being combined, assembly time is 30min；
(3) curing process：Hot pressing temperature is 105 DEG C -115 DEG C, and hot pressing pressure is (1.0 ± 0.1) MPa, and hot pressing time is
1min/mm。
2nd, performance test
(1) bonding strength is determined
According to national standard《GB/T 17657-2013》The II classes glued board gluing strength test method of regulation, in test
State the bonding strength of glued board.Bonding strength is pressed II classes gluing slat element and is processed：Test specimen is placed in the hot water of (63 scholar 3) DEG C and impregnates
3h (should be by test specimen all leaching people's hot water during dipping test specimen), cools down at room temperature 10min and determines again after taking-up.
(2) burst size of methanal is determined
According to national standard《GB/T 17657-2013》The condensed steam water of regulation, tests the Form aldehyde release of above-mentioned glued board
Amount.
(3) measure of water resistance
Glued board is put in boiling water and is boiled, record the time of glued board cracking, the quality of adhesive water resistance can basis
The length of glued board cracking time is being judged.
Embodiment 1：
50 gram 37% of formalin is added in the reactor equipped with agitator, thermometer and reflux condensate device,
Stirring is warming up to 45 DEG C, and it is 5.5 to adjust pH with 5% NaOH solution, adds first urea 20.18g, stirring to be warming up to 85
DEG C, insulation reaction 30min；The NaOH solution regulation pH for adding 5% is 8.5～9.0, adds second batch urea 5.04g, is incubated
30min；Resorcinol 1.35g is added, is incubated after 15min with 20% NH4It is 5.0-5.5 that Cl solution adjusts pH, adds the 3rd
Crowd urea 5.04g, continues to react, and is now drawn in the hot water that glue instills 40 DEG C or so with glue head dropper is continual, when going out
20min is reacted again after existing atomizating phenomenon；The NaOH solution regulation pH for adding 5% is 8.5～9.0, adds the 4th batch of urea
3.36g, after reaction 25min, adds 20% NH4Cl solution adjusts pH to 7.5-8.0, and cooling discharge is obtained urea-formaldehyde resin adhesive
Stick, the technical indicator of urea-formaldehyde resin adhesive is：Free formaldehyde content is 0.06%, and solid content is 56.3%, hardening time
For 186s, viscosity is 52s.
The above-mentioned Lauxite glues of 10g are accurately weighed with 50mL small beakers, 0.1g solid ammonium chlorides is weighed and is added to beaker
In, it is well mixed；Then 3 layers of linden glued board (linden Veneer moisture is 9%) are prepared, double spread amount is 240g/m2, so
Afterwards by the parallel rift grain of two panels examination material to being combined, assembly time is that hot pressing is carried out after 30min, and hot pressing temperature is (110 ± 5)
DEG C, hot pressing pressure is (1.0 ± 0.1) MPa, and hot pressing time is 1min/mm.
According to national standard《GB/T 17657-2013》The II classes glued board gluing strength test method of regulation, in test
The bonding strength of glued board is stated, glued board bonding strength is obtained for 0.80MPa；According to national standard《GB/T 17657-2013》
The condensed steam water of regulation, the burst size of methanal for testing above-mentioned glued board is 0.45mg/L；Glued board is put in boiling water and is boiled, it is glued
The time of plate cracking is 497min.
Embodiment 2：
60 gram 37% of formalin is added in the reactor equipped with agitator, thermometer and reflux condensate device,
Stirring is warming up to 50 DEG C, and it is 5.5 to adjust pH with 5% NaOH solution, adds first urea 26.23g, stirring to be warming up to 88
DEG C, insulation reaction 25min；The NaOH solution regulation pH for adding 5% is 8.5～9.0, adds second batch urea 6.05g, is incubated
25min；Resorcinol 1.61g is added, is incubated after 15min with 20% NH4It is 5.0-5.5 that Cl solution adjusts pH, adds the 3rd
Crowd urea 4.04g, continues to react, and is now drawn in the hot water that glue instills 40 DEG C or so with glue head dropper is continual, when going out
15min is reacted again after existing atomizating phenomenon：The NaOH solution regulation pH for adding 5% is 8.5～9.0, adds the 4th batch of urea
4.04g, after reaction 23min, adds 20% NH4Cl solution adjusts pH to 7.5-8.0, and cooling discharge is obtained urea-formaldehyde resin adhesive
Stick, the technical indicator of prepared urea-formaldehyde resin adhesive is：Free formaldehyde content is 0.06%, and solid content is 57.1%,
Hardening time is 182s, and viscosity is 55s.
The above-mentioned Lauxite glues of 10g are accurately weighed with 50mL small beakers, 0.1g solid ammonium chlorides is weighed and is added to beaker
In, it is well mixed；Then 3 layers of linden glued board (linden Veneer moisture is 10%) are prepared, double spread amount is 245g/m2,
Then by the parallel rift grain of two panels examination material to being combined, assembly time is that hot pressing is carried out after 30min, and hot pressing temperature is (110 ± 5)
DEG C, hot pressing pressure is (1.0 ± 0.1) MPa, and hot pressing time is 1min/mm.
According to national standard《GB/T 17657-2013》The II classes glued board gluing strength test method of regulation, in test
The bonding strength of glued board is stated, glued board bonding strength is obtained for 0.82MPa；According to national standard《GB/T 17657-2013》
The condensed steam water of regulation, the burst size of methanal for testing above-mentioned glued board is 0.42mg/L；Glued board is put in boiling water and is boiled, it is glued
The time of plate cracking is 500min.
Embodiment 3：
55 gram 37% of formalin is added in the reactor equipped with agitator, thermometer and reflux condensate device,
Stirring is warming up to 55 DEG C, and it is 6.5 to adjust pH with 5% NaOH solution, adds first urea 25.16g, stirring to be warming up to 90
DEG C, insulation reaction 20min；The NaOH solution regulation pH for adding 5% is 8.5～9.0, adds second batch urea 5.55g, is incubated
20min；Resorcinol 1.54g is added, is incubated after 15min with 20% NH4It is 5.0-5.5 that Cl solution adjusts pH, adds the 3rd
Urea 3.7g is criticized, continues to react, now drawn in the hot water that glue instills 40 DEG C or so with glue head dropper is continual, work as appearance
React 10min after atomizating phenomenon again；The NaOH solution regulation pH for adding 5% is 8.5～9.0, adds the 4th crowd of urea 2.59g,
After reaction 20min, 20% NH is added4Cl solution adjusts pH to 7.5-8.0, and cooling discharge is obtained urea-formaldehyde resin adhesive, institute
The technical indicator of the urea-formaldehyde resin adhesive of preparation is：Free formaldehyde content is 0.06%, and solid content is 57.5%, hardening time
For 180s, viscosity is 57s.
The above-mentioned Lauxite glues of 10g are accurately weighed with 50mL small beakers, 0.1g solid ammonium chlorides is weighed and is added to beaker
In, it is well mixed；Then 3 layers of linden glued board (linden Veneer moisture is 10%) are prepared, double spread amount is 240g/m2,
Then by the parallel rift grain of two panels examination material to being combined, assembly time is that hot pressing is carried out after 30min, and hot pressing temperature is (110 ± 5)
DEG C, hot pressing pressure is (1.0 ± 0.1) MPa, and hot pressing time is 1min/mm.
According to national standard《GB/T 17657-2013》The II classes glued board gluing strength test method of regulation, in test
The bonding strength of glued board is stated, glued board bonding strength is obtained for 0.81MPa；According to national standard《GB/T 17657-2013》
The condensed steam water of regulation, the burst size of methanal for testing above-mentioned glued board is 0.44mg/L；Glued board is put in boiling water and is boiled, it is glued
The time of plate cracking is 495min.
Examples detailed above technology design only to illustrate the invention and feature, its object is to allow one skilled in the art
Will appreciate that present disclosure and implement according to this, can not be limited the scope of the invention with this.It is all smart according to the present invention
Equivalent transformation or modification that refreshing essence is done, all should be included within the scope of the present invention.
Claims (4)
1. the preparation method of resorcinol modified urea-formaldehyde resin adhesive, it is characterised in that comprise the following steps：
(1) 37% formalin is added equipped with reactor, stirring is warming up to 45～55 DEG C, and the NaOH with 5～10% is molten
It is 5.0～6.5 that liquid adjusts pH, adds first urea, stirring to be warming up to 80～90 DEG C, 20～30min of insulation reaction；
(2) the NaOH solution regulation pH for adding 5～10% is 8.0～9.0, addition second batch urea, insulation reaction 20～
30min；
(3) resorcinol is added, is incubated after 10～15min and adds 15～20% NH4It is 5.0～5.5 that Cl solution adjusts pH, plus
Enter the 3rd batch of urea to continue to react, drawn in the hot water that glue instills 40 DEG C with glue head dropper is continual, it is existing when there is atomization
React 10～20min again as after；
(4) it is 8.0～9.0 that the NaOH solution of addition 5～10% adjusts pH, adds the 4th batch of urea, is added after 20～25min of reaction
Enter 15～20% NH4Cl solution adjusts pH to 7.5～8.0；
(5) when temperature is down to room temperature, filtering and discharging.
2. the preparation method of resorcinol modified urea-formaldehyde resin adhesive according to claim 1, it is characterised in that：Formaldehyde
It is 1.1: 1 with the mol ratio of urea total amount.
3. the preparation method of resorcinol modified urea-formaldehyde resin adhesive according to claim 1 and 2, it is characterised in that：
First urea accounts for the 60～70% of urea total amount in the step (1), and second batch urea accounts for urea total amount in the step (2)
10～15%, the 3rd batch of urea accounts for the 10～15% of urea total amount in the step (3), in the step (4) the 4th batch urine
Element accounts for the 5～10% of urea total amount.
4. the preparation method of resorcinol modified urea-formaldehyde resin adhesive according to claim 3, it is characterised in that：It is described
Resorcinol accounts for the 4～5% of urea total amount in step (3).
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| CN107099268A (en) * | 2017-05-05 | 2017-08-29 | 江苏苏林木业有限公司 | A kind of fibre board use adhesive and preparation method thereof |
| CN108531116B (en) * | 2018-03-19 | 2021-01-15 | 常熟理工学院 | Sulfate lignin modified urea-formaldehyde resin adhesive and preparation method thereof |
| CN110903451A (en) * | 2019-11-21 | 2020-03-24 | 书香门地（上海）美学家居股份有限公司 | Preparation method of urea-formaldehyde resin with high prepressing performance and low molar ratio |
| CN113429536A (en) * | 2021-07-02 | 2021-09-24 | 景谷慧通木业有限责任公司 | Preparation method of E0-grade urea-formaldehyde resin for environment-friendly plywood |
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| CN101475676B (en) * | 2009-01-20 | 2011-06-29 | 江苏工业学院 | Preparation of urea-formaldehyde resin for environment-friendly artificial board |
| CN102086295B (en) * | 2010-06-28 | 2013-05-08 | 永港伟方（北京）科技股份有限公司 | Urea-formaldehyde resin for non-dewatering particleboard and preparation method thereof |
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