CN108822275A - A kind of quick-setting low mole prop0rtion modified urea-formaldehyde resin preparation method of ecological board cold pressing - Google Patents
A kind of quick-setting low mole prop0rtion modified urea-formaldehyde resin preparation method of ecological board cold pressing Download PDFInfo
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- CN108822275A CN108822275A CN201810755123.4A CN201810755123A CN108822275A CN 108822275 A CN108822275 A CN 108822275A CN 201810755123 A CN201810755123 A CN 201810755123A CN 108822275 A CN108822275 A CN 108822275A
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- urea
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/40—Chemically modified polycondensates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08G12/34—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds and acyclic or carbocyclic compounds
- C08G12/36—Ureas; Thioureas
- C08G12/38—Ureas; Thioureas and melamines
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention discloses a kind of ecological boards to be cold-pressed quick-setting low mole prop0rtion modified urea-formaldehyde resin.Furthermore, the invention also discloses the synthetic methods of the quick-setting low mole prop0rtion modified urea-formaldehyde resin of cold pressing, the method is using aldehyde compound and urea as primary raw material, it is modified in Lauxite synthesis process using melamine, toughener and reinforcing agent, using aldehyde compound and the secondary polycondensating process of urea, increase in Lauxite viscosity and molecular weight while improving Lauxite condensation depth, enable the Lauxite of preparation to realize rapid curing and low burst size of methanal at normal temperature, can be used for being cold-pressed the manufacturing field of overlaid wood based panel.
Description
Technical field
The present invention relates to a kind of Lauxite synthetic methods, and in particular to a kind of quick-setting low mole prop0rtion of cold pressing is modified
Preparation of urea-formaldehyde resin.
Background technique
Lauxite molecule makes after solidification poor water resistance in Lauxite compared with strongly hydrophilic due to having, and there are glue
Layer is more crisp, be easily cracked, methylol and methylene ether link decompose so that artifical plate product in loss of properties on aging and Lauxite
The disadvantages of burst size of methanal is high is subject to certain restrictions the application range of Lauxite, therefore melamine modified urea can be used
Urea formaldehyde improves water resistance, improves glue-line brittleness, using reinforcing agent raising bonding strength using plasticizer is modified, obtains formaldehyde and releases
It is high-volume low, glue performance is excellent, flexibility is preferable and room temperature is cold-pressed quick-setting environment protection type urea formaldehyde resin.
Summary of the invention
For the above-mentioned existing prior art, the present invention provides a kind of quick-setting low mole prop0rtion modified urea-formaldehyde resin of cold pressing
The free formaldehyde release in resin can be effectively reduced in preparation method, this method, and improve resin glue performance and glue-line it is soft
Toughness and room temperature are cold-pressed curing rate.
In order to achieve the above object, the technical scheme adopted by the invention is that：There is provided that a kind of cold pressing is quick-setting low to rub
, than modified urea-formaldehyde resin preparation method, this method successively includes the following steps for you：
(1) it dissolves by heating and carries out addition reaction：Using heating and alkaline condition（pH=7~8）By urea, toughener and aldehydes chemical combination
Object is sufficiently dissolved, is uniformly mixed, and addition reaction, reaction time about 1h are then carried out under 90 DEG C of constant temperatures；
(2) low molecular weight urea resin prepolymer synthesizes：Using acid condition（pH=5~6）By step（1）Urea, toughener
It is sufficiently reacted with aldehyde mixture, reaction time about 1h, reaction temperature is 90 DEG C；It can stop after viscosity needed for be achieved anti-
It answers；
(3) melamine, urea and reinforcing agent modified urea-formaldehyde resin performed polymer are utilized：Using alkaline condition（pH=7~8）By second
Aldehyde mixture and urea are criticized, step is added in a certain amount of melamine and reinforcing agent（2）Hybrid resin in, reaction temperature is
90 DEG C, resin mixture liquor is adjusted to acidity after urea and melamine are completely dissolved about 30min（pH=5~6）, reaction to institute
Need viscosity；
(4) free formaldehyde content is reduced using urea：In step（3）After the completion, in alkaline condition（pH=7~8）It is lower to criticize third
Urea, which is added in resin, reduces free formaldehyde content, reaction time about 30min, and reaction temperature is 90 DEG C, then cooling discharging.
The beneficial effects of the invention are as follows：By adding toughener, Lauxite cured glue layer brittleness is improved；It is secondary
After polycondensation, the free formaldehyde of resin system is substantially reduced；Modified using melamine and reinforcing agent, resinoid bond is dry, wet glue
Than one time resulting modified urea-formaldehyde resin of polycondensation of intensity is closed obviously to rise.Meanwhile utilizing melamine, reinforcing agent modified urea-formaldehyde tree
Rouge performed polymer can make the performance of ureaformaldehyde condensation polymer obtain good improvement while increasing the initial stage adhesion strength of resin, can be real
Existing room temperature is cold-pressed rapid curing.
Based on the above technical solution, the present invention can also be improved as follows：
Further, first stage alkalinity is pH=7.5 in step (1), and reaction temperature is 95 DEG C, reaction time 45min；
Further, acid in step (2) is pH=5.5, and reaction temperature is 95 DEG C, reaction time 30min；
Further, step (3) neutral and alkali is pH=7.5, and reaction temperature is 95 DEG C, reaction time 30min；Acidity is pH=4.5,
Reaction temperature is 95 DEG C, reaction time 20min；
Further, step (4) neutral and alkali is pH=7.5, and reaction temperature is 95 DEG C, reaction time 25min；
Above-mentioned parameter is preferred parameter, and under its parameter, modified environment protection type urea formaldehyde resin synthesis process presentation property is most complete, reaction
Fastest, resinoid bond intensity highest, burst size of methanal are minimum, room temperature cold pressing solidification is most fast.
Specific embodiment
Specific embodiments of the present invention will be described in detail below.
In the embodiment of the present invention, a kind of cold pressing quick-setting low mole prop0rtion modified urea-formaldehyde resin synthesis side is provided
Method including toughening agent modified low molecular weight urea resin prepolymer synthesis, utilizes melamine, urea and reinforcing agent modified urea
Urea formaldehyde performed polymer and etc..
Urea, toughener and aldehyde compound are synthesized into low molecular weight Lauxite first：By aldehyde compound 50 ~ 60
In part, 15 ~ 25 parts of urea, 0.5~5 part of toughener and 5 ~ 10 parts of addition three-necked flasks of basic catalyst, in alkaline condition（pH=
7.0~8.0）Be warming up to 95 DEG C and keep the temperature a period of time amount to 45min, so as to generate cross-linking reaction one hydroxyl of main compound, two
Hydroxyl and trimethylol urea；It is subsequently added into 0.5 ~ 1 part of acidic catalyst, the pH value of reactant is adjusted to acidity（pH=4.5~5.5）,
Reaction temperature is 95 DEG C, and the low molecular weight ureaformaldehyde tree that polycondensation reaction is tentatively crosslinked sufficiently occurs for the reactant to the first stage
Rouge performed polymer, reaction time are about 25 ~ 30min；Second stage uses basic catalyst by resin compound tune after completion of the reaction
For alkalinity（pH=7.0~8.0）, reaction temperature is 95 DEG C, by 5 ~ 10 parts of second batch aldehyde compound, 5 ~ 10 parts of urea, melamine
5~10 parts of amine and 0.5~5 part of reinforcing agent are slowly added to reaction kettle the reaction was continued 30min.Then utilize acidic catalyst by resin
Mixture is adjusted to acidity（pH=5.0~5.5）, allow low molecular weight urea resin prepolymer and melamine, urea, reinforcing agent and aldehyde
The reticular structure that polycondensation reaction forms high density crosslinking, the elementary reaction time about 25 ~ 30min occur for class mixture.It is to appear
Polycondensation reaction is terminated using basic catalyst after flocculent deposit, then urea 5-10 parts of addition, anti-with the free formaldehyde in resin
Answer cooling discharging after 30min.The final solid content of resin that this example obtains is 55% or so, and initial viscosity is 30 ~ 37mPa.s,
Free formaldehyde content is 0.22%-0.38%.
Using above-mentioned secondary polycondensation and the secondary adding method of aldehyde compound, viscosity is preferable, bonding strength is high at the beginning of capable of obtaining,
Free formaldehyde content is low, glued board burst size of methanal is low, room temperature is cold-pressed quick-setting environment-friendly modified Lauxite.
The following examples are only intended to that the present invention will be described in detail, do not limit the range of invention in any way.
(1) embodiment one
Present embodiment uses 60 parts of formaldehyde, 33 parts of urea, 3 parts of 6 parts of toughener, 8 parts of melamine and reinforcing agent synthesizing environment-friendlies
Type modified urea-formaldehyde resin, specific step is as follows：
Addition reaction is carried out 1. dissolving by heating：Using heating and alkaline condition（pH=7.5）Urea, toughener and formaldehyde are dissolved
And 1h is reacted under 90 DEG C of constant temperatures after mixing；
2. low molecular weight urea resin prepolymer synthesizes：Using acid condition（pH=5.5）By step（1）The methylolurea of generation
It is sufficiently reacted under the conditions of 90 DEG C, can stop reacting when smoke-like cloud point occurs in viscosity, the elementary reaction time is about
30min；
3. in alkaline condition（pH=8.0）By second batch formaldehyde and urea, mixing is added in a certain amount of melamine and reinforcing agent
In resin, reaction temperature is 90 DEG C, and resin mixture liquor is adjusted to acidity after heating 30min（pH=5.0）, react and extremely sink
Shallow lake formula cloud point, is adjusted to alkalinity for resin solution immediately（pH=8.0）；
4. resin solution and reaction time 30min is added in third batch urea, reaction temperature is 90 DEG C, then cooling discharging；
5. the specific data of precuring Lauxite molecular weight obtained by present embodiment are as follows：
(2) embodiment two
Present embodiment uses 58 parts of formaldehyde, 32 parts of urea, 3.5 parts of 4 parts of toughener, 7 parts of melamine and reinforcing agent synthesis rings
Guarantor's type modified urea-formaldehyde resin, specific step is as follows：
Addition reaction is carried out 1. dissolving by heating：Using heating and alkaline condition（pH=8.0）Urea and formaldehyde are dissolved and mixed
50min is reacted under 95 DEG C of constant temperatures after even；
2. low molecular weight urea resin prepolymer synthesizes：Using acid condition（pH=5.0）By step（1）The methylolurea of generation
It is sufficiently reacted under the conditions of 95 DEG C, can stop reacting when smoke-like cloud point occurs in viscosity, the elementary reaction time is about
20min；
3. in alkaline condition（pH=8.0）By second batch formaldehyde and urea, compound tree is added in a certain amount of melamine and reinforcing agent
In rouge, reaction temperature is 95 DEG C, and resin mixture liquor is adjusted to acidity after heating 30min（pH=4.5）, reaction is to precipitating
Formula cloud point, is adjusted to alkalinity for resin solution immediately（pH=8.0）；
4. resin solution and reaction time 30min is added in third batch urea, reaction temperature is 95 DEG C, then cooling discharging.
5. the specific data of precuring Lauxite molecular weight obtained by present embodiment are as follows：
Claims (5)
1. being cold-pressed quick-setting low mole prop0rtion modified urea-formaldehyde resin, which is characterized in that resin raw material formula is in terms of mass parts, group
Become：
45~55 parts of urea
55~65 parts of aldehyde compound
2~5 parts of melamine
5~20 parts of basic catalyst
0.5~5 part of acidic catalyst
0.5~5 part of reinforcing agent
0.5~5 part of toughener
（1）Low molecular weight urea resin prepolymer：Using alkali-acid technique by urea, aldehyde compound, toughener, through addition and
Low molecular weight urea resin prepolymer is synthesized after polycondensation reaction, stops polycondensation reaction after obtaining required molecular weight；
（2）Melamine and reinforcing agent modified low molecular weight urea resin prepolymer：Use alkali-acid technique with melamine and increasing
Strong agent at high temperature with step（1）Performed polymer stir evenly under alkaline condition, carry out polycondensation reaction in acid condition, when
Stop polycondensation reaction after obtaining required molecular weight；
（3）Free formaldehyde content in resin is reduced using urea：Step is reduced using urea under the conditions of high-temperature alkaline（2）Synthesis
High molar ratio modified urea-formaldehyde resin, the slow cooling after urea is completely dissolved, and will the environment-friendly modified ureaformaldehyde that finishes of synthesis
Resin is adjusted to the cooling taking-up of alkalinity.
2. the quick-setting low mole prop0rtion modified urea-formaldehyde resin of cold pressing according to claim 1, it is characterized in that：The aldehydes
Compound is any one in paraformaldehyde, acetaldehyde, furfural or salicylide.
3. the quick-setting low mole prop0rtion modified urea-formaldehyde resin of cold pressing according to claim 1, it is characterized in that：Base catalysis
Agent is any one in sodium hydroxide, potassium hydroxide, barium hydroxide, sodium carbonate, potassium carbonate or calcium oxide.
4. the quick-setting low mole prop0rtion modified urea-formaldehyde resin of cold pressing according to claim 1, it is characterized in that：Acidic catalyst
Agent is any one in formic acid, hydrochloric acid, ammonium chloride, ammonium persulfate or ammonium sulfate.
5. it is cold-pressed quick-setting low mole prop0rtion modified urea-formaldehyde resin, it is characterized in that：Successively include the following steps：
（1）It dissolves by heating and carries out addition reaction：Toughener, urea and aldehyde compound are dissolved using 90 DEG C of water-baths,
It is adjusted between alkalinity；
（2）Performed polymer synthesis：It is adjusted between acidity after wait keep the temperature, stops reaction after reaction to required viscosity；
（3）Utilize melamine, urea and reinforcing agent modified urea-formaldehyde resin performed polymer：Under alkaline condition by melamine,
Urea and reinforcing agent are added in performed polymer to react is adjusted to acidity after a certain period of time, reaction to required viscosity；
（4）Free formaldehyde content is reduced using urea：In step（3）After the completion, urea is added in resin under alkaline condition
Reduce free formaldehyde content.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810755123.4A CN108822275A (en) | 2018-07-11 | 2018-07-11 | A kind of quick-setting low mole prop0rtion modified urea-formaldehyde resin preparation method of ecological board cold pressing |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810755123.4A CN108822275A (en) | 2018-07-11 | 2018-07-11 | A kind of quick-setting low mole prop0rtion modified urea-formaldehyde resin preparation method of ecological board cold pressing |
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| CN108822275A true CN108822275A (en) | 2018-11-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810755123.4A Pending CN108822275A (en) | 2018-07-11 | 2018-07-11 | A kind of quick-setting low mole prop0rtion modified urea-formaldehyde resin preparation method of ecological board cold pressing |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0323778A1 (en) * | 1987-12-23 | 1989-07-12 | Elf Atochem S.A. | Process for the fabrication of urea-formaldehyde resins containing melamine |
-
2018
- 2018-07-11 CN CN201810755123.4A patent/CN108822275A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0323778A1 (en) * | 1987-12-23 | 1989-07-12 | Elf Atochem S.A. | Process for the fabrication of urea-formaldehyde resins containing melamine |
Non-Patent Citations (2)
| Title |
|---|
| 李明: "低摩尔比高醚三聚氰胺改性脲醛树脂合成、结构及性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 赵立: "《新型材料在家具工业中的应用》", 31 December 1986, 轻工业出版社 * |
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Application publication date: 20181116 |