CN100999652A - Preparation process of urea-formaldehyde resin adhesive - Google Patents

Preparation process of urea-formaldehyde resin adhesive Download PDF

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Publication number
CN100999652A
CN100999652A CN 200610171037 CN200610171037A CN100999652A CN 100999652 A CN100999652 A CN 100999652A CN 200610171037 CN200610171037 CN 200610171037 CN 200610171037 A CN200610171037 A CN 200610171037A CN 100999652 A CN100999652 A CN 100999652A
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China
Prior art keywords
urea
formaldehyde resin
liquid
resin adhesive
preparation
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CN 200610171037
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CN100439463C (en
Inventor
褚宏春
吕运江
吴章
孔凡玲
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National Engineering Research Center Of Watered Coal Slurry Gasification And Coa
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National Engineering Research Center Of Watered Coal Slurry Gasification And Coa
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Abstract

The present invention is process of preparing urea-formaldehyde resin adhesive. The preparation process includes the following steps: 1. adding formaldehyde in 420-600 weight portions into a reaction kettle and regulating pH value to 7.0-9.0 with alkali; 2. adding liquid urea from a urea synthesizing apparatus in 185-395 weight portions into the reaction kettle, reaction at 90-95 deg.c for 0.5-1.5 hr, regulating pH value to 4.0-5.5 with acid and further reaction until the solution becomes turbid and has viscosity of 15-20 CP; 3. regulating pH value to 7.0-7.6 with alkali and adding liquid urea of other 10-15 weight portions; 4. decompression dewatering, adding liquid urea of other 5-10 weight portions and modifier of 3-30 weight portions at temperature not higher than 70 deg.c and absolute pressure of 0.08-0.19 atm; and 5. regulating pH value to 7.5-8.5 with alkali, cooling to below 50 deg.c, discharging and packing.

Description

A kind of preparation method of urea-formaldehyde resin adhesive
Technical field:
The present invention relates to a kind of tackiness agent, relate to a kind of preparation method of urea-formaldehyde resin adhesive concretely.
Background technology:
Urea-formaldehyde resin adhesive is a kind of consolidation strength height, tackiness agent water-fast, heat-resisting, with low cost, is widely used in the bonding of wood working industry, paper product and other material.Owing to using urea-formaldehyde resin or using in the product process for preparing by urea-formaldehyde resin adhesive, the formaldehyde that discharges stimulates people's eyes and respiratory system, serious environment pollution, the harm people's is healthy, standard has all been formulated one after another to the free formaldehyde content of urea-formaldehyde resin and goods thereof in countries in the world, relevant technologies expert has done a lot of discussions, has proposed many technical schemes.
At present, urea-formaldehyde resin preparation technology generally is to be raw material with urea and formaldehyde, and needs in the urea-formaldehyde resin preparation process with steam heating, control certain temperature.And the finishing operation of urea production is that fused urea-urea liquid is sprayed granulation, and in granulation process, urea liquid is cured near room temperature from more than 100 ℃ of landing at the prilling tower top, and the heat that this urea liquid contains can't be recycled.In addition, complex process, energy consumption is big, the cost height.
Summary of the invention
Purpose of the present invention is intended to overcome the deficiencies in the prior art, providing a kind of is raw material with the urea liquid of urea plant production directly, effectively utilizes the technology of urea liquid heat simple, the preparation method of the urea-formaldehyde resin adhesive of save energy, reduction labour intensity and cost.
Purpose of the present invention can realize by following technical measures:
This method is carried out as follows:
(1). the formaldehyde of 420-600 weight part is added in the reactor, with adjusting PH with base=7.0-9.0;
(2). slowly in reactor, add the liquid urea liquid of the 185-395 weight part of carrying by apparatus for urea synthesis, when temperature of reaction is 90~95 ℃, be incubated 0.5-1.5 hour, pH=4.0-5.5 is transferred with acid in the back, continue to react to the solution becomes muddiness, viscosity is 15-20CP;
(3). with adjusting PH with base=7.0-7.6, and then adding is by the liquid urea liquid of the 10-15 weight part of apparatus for urea synthesis conveying;
(4). decompression dehydration controlled temperature≤70 ℃, when absolute pressure is 0.08-0.19 normal atmosphere, adds the liquid urea liquid of the 5-10 weight part of being carried by apparatus for urea synthesis at last, and adds the properties-correcting agent of 3-30 weight part;
(5). with adjusting PH with base=7.5-8.5, when being cooled to tackiness agent temperature in the reactor≤50 ℃, discharging, pack product.
Purpose of the present invention also can realize by following technical measures:
Described acid comprises formic acid, acetate, hydrochloric acid, sulfuric acid, nitric acid or ammonium chloride; Described alkali comprises sodium hydroxide, potassium hydroxide or ammoniacal liquor; Described properties-correcting agent comprises trimeric cyanamide, polyvinyl alcohol or thiocarbamide; Add the polysiloxane surfactant of 0.1-1.0% before the discharging, spraying drying can obtain the powdery solid urea-formaldehyde resin then.
Raw material formaldehyde of the present invention, its weight concentration are 37%.The outward appearance of the product of the present invention thick liquid that is creamy white.
The present invention is the raw material production urea-formaldehyde resin with urea liquid, utilize the waste heat of urea liquid to give the heating of urea-formaldehyde resin reactive system, saved the steam that urea-formaldehyde resin production needs, reduced the urea product Packing Unit simultaneously, reduce the production cost of urea-formaldehyde resin, improved the competitive edge of urea-formaldehyde resin product.
The technical solution used in the present invention is to introduce one to the urea-formaldehyde resin reactor from the urea liquid that removes shower nozzle, control the adding quantity and the flow of urea liquid by valve, under meter or scale tank, add-on and speed with urea liquid realize adding thermal control, can effectively reduce even eliminate fully the situation that needs to use thermals source such as steam in traditional urea-formaldehyde resin production process.
Because the production process of urea-formaldehyde resin is used external steam hardly, the manufacturing cost of urea liquid is lower than the cost of buying granular urea, and cancelled the operation that in the urea-formaldehyde resin production granular urea is melt into urea liquid, technology is simple, make the urea-formaldehyde resin production cost that obvious decline be arranged, because the biuret that the required urea liquid of production urea-formaldehyde resin requires is not strict, make urea-urea liquid production more easy to operate in addition.
Embodiment
Embodiment 1:
(1). 420Kg formaldehyde is added in the reactor, with sodium hydroxide solution adjust pH to 9.0;
(2). open the urea fluid valve, slowly in reactor, add first the liquid urea liquid 185Kg that carries by apparatus for urea synthesis and finish temperature of reaction in the time of 95 ℃, insulation reaction 0.5h, PH=5.5 is regulated with ammonium chloride solution in the back, continue to react to the solution becomes muddiness, viscosity is 15CP;
(3). transfer pH=7.6 with sodium hydroxide solution, and then add the second crowd of liquid urea liquid 10Kg that carries by apparatus for urea synthesis;
(4). decompression dehydration, controlled temperature are at 50 ℃, and absolute pressure is 0.19 normal atmosphere, when viscosity is 5CP, adds the 3rd crowd of liquid urea liquid 10Kg that is carried by apparatus for urea synthesis at last, and adds trimeric cyanamide 3kg;
(5). with adjusting PH with base=8.5, be cooled to discharging when the tackiness agent temperature is 40 ℃ in the reactor, pack product.
Embodiment 2:
(1). 600Kg formaldehyde is added in the reactor, with sodium hydroxide solution adjust pH to 7.0;
(2). open the urea fluid valve, slowly in reactor, add first the liquid urea liquid 395Kg that carries by apparatus for urea synthesis, finish temperature of reaction in the time of 90 ℃, insulation reaction 1.5h, PH=4.0 is regulated with ammonium chloride solution in the back, continues to react to the solution becomes muddiness, and viscosity is 20CP;
(3). transfer pH=7.0 with sodium hydroxide solution, and then add the second crowd of liquid urea liquid 15Kg that carries by apparatus for urea synthesis;
(4). decompression dehydration, controlled temperature are at 70 ℃, and absolute pressure is 0.08 normal atmosphere, when viscosity is 500CP, adds the 3rd crowd of liquid urea liquid 5Kg that is carried by apparatus for urea synthesis at last, and adds trimeric cyanamide 30kg;
(5). with adjusting PH with base=7.5, be cooled to discharging when the tackiness agent temperature is 40 ℃ in the reactor, pack product.
Embodiment 3:
(1). 500Kg formaldehyde is added in the reactor, with sodium hydroxide solution adjust pH to 8.0;
(2). open the urea fluid valve, slowly in reactor, add first the liquid urea liquid 280Kg that carries by apparatus for urea synthesis, finish temperature of reaction in the time of 92 ℃, insulation reaction 1h, PH=4.5 is regulated with ammonium chloride solution in the back, continues to react to the solution becomes muddiness, and viscosity is 18CP;
(3). transfer pH=7.3 with sodium hydroxide solution, and then add the second crowd of liquid urea liquid 12Kg that carries by apparatus for urea synthesis;
(4). decompression dehydration, controlled temperature are at 60 ℃, and absolute pressure is 0.13 normal atmosphere, when viscosity is 250CP, adds the 3rd crowd of liquid urea liquid 8Kg that is carried by apparatus for urea synthesis at last, and adds trimeric cyanamide 15kg;
(5). with adjusting PH with base=8.0, be cooled to when the tackiness agent temperature is 45 ℃ in the reactor, add 0.5% polysiloxane surfactant, mist projection granulating discharging behind the mixing, pack powder-like product.
Embodiment 4:
With embodiment 1,2,3, different is that described ammonium chloride substitutes with formic acid, acetate, hydrochloric acid, sulfuric acid or nitric acid respectively respectively.
Embodiment 5:
With embodiment 1,2,3,4, different is that described trimeric cyanamide substitutes with polyvinyl alcohol or thiocarbamide respectively respectively.
Embodiment 6:
With embodiment 1,2,3,4,5, different is that described sodium hydroxide substitutes with potassium hydroxide or ammoniacal liquor respectively respectively.

Claims (5)

1, a kind of preparation method of urea-formaldehyde resin adhesive is characterized in that this method carries out as follows:
(1). the formaldehyde of 420-600 weight part is added in the reactor, with adjusting PH with base=7.0-9.0;
(2). slowly in reactor, add the liquid urea liquid of the 185-395 weight part of carrying by apparatus for urea synthesis, when temperature of reaction is 90~95 ℃, be incubated 0.5-1.5 hour, pH=4.0-5.5 is transferred with acid in the back, continue to react to the solution becomes muddiness, viscosity is 15-20CP;
(3). with adjusting PH with base=7.0-7.6, and then adding is by the liquid urea liquid of the 10-15 weight part of apparatus for urea synthesis conveying;
(4). decompression dehydration controlled temperature≤70 ℃, when absolute pressure is 0.08-0.19 normal atmosphere, adds the liquid urea liquid of the 5-10 weight part of being carried by apparatus for urea synthesis at last, and adds the properties-correcting agent of 3-30 weight part;
(5). with adjusting PH with base=7.5-8.5, when being cooled to tackiness agent temperature in the reactor≤50 ℃, discharging, pack product.
2,, it is characterized in that described acid comprises formic acid, acetate, hydrochloric acid, sulfuric acid, nitric acid or ammonium chloride according to the preparation method of claims 1 described a kind of urea-formaldehyde resin adhesive.
3,, it is characterized in that described alkali comprises sodium hydroxide, potassium hydroxide or ammoniacal liquor according to the preparation method of claims 1 described a kind of urea-formaldehyde resin adhesive.
4,, it is characterized in that described properties-correcting agent comprises trimeric cyanamide, polyvinyl alcohol or thiocarbamide according to the preparation method of claims 1 described a kind of urea-formaldehyde resin adhesive.
5, according to the preparation method of claims 1 described a kind of urea-formaldehyde resin adhesive, it is characterized in that the polysiloxane surfactant of the preceding 0.1-1.0% of adding of discharging, spraying drying can obtain the powdery solid urea-formaldehyde resin then.
CNB2006101710376A 2006-12-31 2006-12-31 Preparation process of urea-formaldehyde resin adhesive Expired - Fee Related CN100439463C (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102220100A (en) * 2011-05-25 2011-10-19 三明学院 Low-toxicity urea formaldehyde resin adhesive and preparation method thereof
CN101555396B (en) * 2009-05-12 2012-01-25 张文通 Production method of urea-formaldehyde resin adhesive
CN103192441A (en) * 2013-04-19 2013-07-10 琚长林 Plant fiber composite fireproof plate
CN103203791A (en) * 2013-04-24 2013-07-17 琚长林 Novel environment-friendly plant fiber home door
CN104760101A (en) * 2015-03-30 2015-07-08 广西宾阳县荣良新材料科技有限公司 Production method of flame-retardant modified wood
CN104924388A (en) * 2014-10-16 2015-09-23 洋浦久聚台木材科技有限公司 Wood modification working liquid used for wet plate processing and use method thereof
CN105348463A (en) * 2015-12-07 2016-02-24 广西南宁德源胶粘剂有限公司 Preparation method for E2-grade building template glue
CN105346178A (en) * 2015-10-28 2016-02-24 陕西理工学院 Plant fiber-urea formaldehyde resin environment-friendly composite board and preparation method thereof
CN107268331A (en) * 2017-07-25 2017-10-20 攀枝花学院 Impregnate paper glue modifying agent and preparation method thereof
CN108687887A (en) * 2018-04-23 2018-10-23 太尔化工(南京)有限公司 A kind of preparation method and application of solid-state bloom melamine-impregnated decorative paper
CN109651576A (en) * 2019-02-18 2019-04-19 贵州中宝装饰材料有限公司 Compound and application preparation of the tourmaline in Lauxite
CN110936461A (en) * 2019-12-09 2020-03-31 陕西理工大学 Preparation process of bamboo shoot shell-urea resin laminated plate

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US9346926B2 (en) * 2013-03-14 2016-05-24 Georgia-Pacific Chemicals Llc High flow urea-formaldehyde powders for particleboard and fiberboard manufacture

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2433680A (en) * 1944-05-19 1947-12-30 Backman Ove Emil Method of making adhesive film
CN1105694A (en) * 1994-08-22 1995-07-26 山河屯林业局木材综合加工厂 Melamine urea-formaldehyde resin non-dehydrated glue and its production method
CN1291632A (en) * 2000-09-21 2001-04-18 何卫平 Low-poison urea-formaldehyde resin adhesive and its preparing process

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101555396B (en) * 2009-05-12 2012-01-25 张文通 Production method of urea-formaldehyde resin adhesive
CN102220100B (en) * 2011-05-25 2013-04-03 三明学院 Low-toxicity urea formaldehyde resin adhesive and preparation method thereof
CN102220100A (en) * 2011-05-25 2011-10-19 三明学院 Low-toxicity urea formaldehyde resin adhesive and preparation method thereof
CN103192441A (en) * 2013-04-19 2013-07-10 琚长林 Plant fiber composite fireproof plate
CN103203791A (en) * 2013-04-24 2013-07-17 琚长林 Novel environment-friendly plant fiber home door
CN103203791B (en) * 2013-04-24 2015-09-09 琚长林 A kind of string house ornamentation door
CN104924388A (en) * 2014-10-16 2015-09-23 洋浦久聚台木材科技有限公司 Wood modification working liquid used for wet plate processing and use method thereof
CN104760101A (en) * 2015-03-30 2015-07-08 广西宾阳县荣良新材料科技有限公司 Production method of flame-retardant modified wood
CN105346178B (en) * 2015-10-28 2018-05-01 陕西理工学院 A kind of plant fiber-Lauxite Environment-friendlycomposite composite board and preparation method thereof
CN105346178A (en) * 2015-10-28 2016-02-24 陕西理工学院 Plant fiber-urea formaldehyde resin environment-friendly composite board and preparation method thereof
CN105348463A (en) * 2015-12-07 2016-02-24 广西南宁德源胶粘剂有限公司 Preparation method for E2-grade building template glue
CN107268331A (en) * 2017-07-25 2017-10-20 攀枝花学院 Impregnate paper glue modifying agent and preparation method thereof
CN108687887A (en) * 2018-04-23 2018-10-23 太尔化工(南京)有限公司 A kind of preparation method and application of solid-state bloom melamine-impregnated decorative paper
CN109651576A (en) * 2019-02-18 2019-04-19 贵州中宝装饰材料有限公司 Compound and application preparation of the tourmaline in Lauxite
CN110936461A (en) * 2019-12-09 2020-03-31 陕西理工大学 Preparation process of bamboo shoot shell-urea resin laminated plate
CN110936461B (en) * 2019-12-09 2022-03-29 陕西理工大学 Preparation process of bamboo shoot shell-urea resin laminated plate

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