CN104212122A - Additive of phenolic resin as well as preparation method and application of additive - Google Patents

Additive of phenolic resin as well as preparation method and application of additive Download PDF

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Publication number
CN104212122A
CN104212122A CN201410442667.7A CN201410442667A CN104212122A CN 104212122 A CN104212122 A CN 104212122A CN 201410442667 A CN201410442667 A CN 201410442667A CN 104212122 A CN104212122 A CN 104212122A
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additive
resol
phenolic resin
mixture
cake
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CN201410442667.7A
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CN104212122B (en
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范东斌
储富祥
李改云
秦特夫
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Research Institute of Wood Industry of Chinese Academy of Forestry
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Research Institute of Wood Industry of Chinese Academy of Forestry
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Abstract

The invention discloses an additive of phenolic resin as well as a preparation method and an application of the additive, and belongs to the field of wood adhesives. The additive mainly comprises oil-tea-cake, a crosslinking agent, a curing accelerator, a stabilizer and water. The preparation method comprises the following steps: evenly dispersing oil-tea-cake powder into water; adding the crosslinking agent and evenly stirring; carrying out thermal reaction at 50-70 DEG C for 2-3 hours, and cooling to 30 DEG C; and adding the curing accelerator and the stabilizer, evenly stirring and carrying out thermal reaction for 0.5-1 hour, so as to obtain the additive of the phenolic resin, wherein the additive is applied to an adhesive of the phenolic resin. The curing speed and the bonding strength of the adhesive of the phenolic resin can be effectively improved, the hot-pressing time of plywood is shortened, and the hydrolytic resistance of the plywood can be significantly improved, and thus the production efficiency is improved, and the energy consumption and the manufacturing cost are reduced. The additive of the phenolic resin has social significances of energy conservation and emission reduction, and the preparation method is simple, and convenient to operate.

Description

A kind of additive, preparation method and application of resol
Technical field
The present invention relates to a kind of additive, preparation method and application of resol, be specifically related to additive, the preparation method of a kind of wood-based plate resol and contain described additive application in phenolic resin adhesive, belong to based Wood Adhesives field.
Background technology
Resol (PF resin) is to realize the earliest in the world industrialized synthetic resins, mainly for the manufacture of various plastics, coating, tackiness agent, synthon, fire-retardant material etc., is very important macromolecular material.Resol has high, the resistance to boiling water of Joint strength, heat-resisting, weather-proof as tackiness agent, and the advantages such as resistance to chemical attack, are widely used in wood processing field, is the conventional tackiness agent of outdoor structure wood-based plate.In recent years, along with building, the increase of transport field to engineering materials demands such as oriented wood chipboard, cord-wood, container bottom boards, the market outlook of outdoor wood-based plate are very wide, the annual production of PF resin is increased year by year, be increased to 650,000 t of 2013 from 260,000 t of 2007, amplification has shown wide development space up to 150%, PF resin.But, expensive due to phenol, the price that makes resol all the time according to height not under, and resol self also exists some shortcomings, as firmly crisp in the glue-line after solidifying, easily be full of cracks, particularly curing speed is slower compared with other aminoresin, and these have caused the price of resol splicing goods relatively high, production efficiency is not high, have limited synvaren and have applied widely.
By add low cost material in resol, reduce the cost of resol, have great importance for the Application Areas that expands resol.Conventionally adopt bean powder, degreasing soybean protein powder and flour etc. to reduce the cost of resol, still because these materials are raw materials of some agricultural and sideline food, price is higher, and the amplitude that therefore reduces resol cost is very limited.And the shortcoming such as the interpolation of these materials usually can cause the set time of resol long, Joint strength is low, working life is short, usability is poor.In resol, add the curing speed that can improve resin carbonate such as sodium carbonate, but can cause the shortcoming such as reduction working life, bonding strength attenuating of resin.
Summary of the invention
For above-mentioned defect, one of object of the present invention is to provide a kind of additive of resol, and described additive is cheap, reactive behavior is high, can significantly reduce the cost of resol, increases substantially curing speed and the bonding strength of resol.Two of object is to provide a kind of preparation method of additive of resol, and described method is simple, easy and simple to handle;
The object of the invention is to be achieved through the following technical solutions.
An additive for resol, taking described additive total mass as 100%, each component and quality percentage composition are as follows:
Wherein, cake of camellia oleifera seeds is residual solid matter after the Extraction oil of seed tea-seed oil of oil tea (Camellia oleifera), and taking cake of camellia oleifera seeds total mass as 100%, camellia seed oil content is less than 10%, and the granularity of cake of camellia oleifera seeds is less than 200 orders;
The preferred cyanurotriamide modified urea resin performed polymer of linking agent, its preparation method is as follows:
Urea, formaldehyde and trimeric cyanamide are mixed, add formic acid, stir; Be heated to 85 DEG C, insulation is 12~15 seconds to being coated with 4 viscosity, is cooled to 70 DEG C, adds sodium hydroxide solution, adjust pH to 7.5, and reaction 15min, is cooled to 30 DEG C, and discharging, obtains described cyanurotriamide modified urea resin performed polymer;
Wherein, the preferred 1:1.3:0.05:0.01 of the mass ratio of described urea, formaldehyde, trimeric cyanamide and formic acid;
In sodium hydroxide solution, the massfraction of sodium hydroxide is 30%;
More than one in the preferred sodium carbonate of curing catalyst, glycerol acetate and propylene carbonate;
More than one in stablizer preferably phosphoric acid sodium dihydrogen, Sodium phosphate dibasic, borax and Sodium Benzoate;
A preparation method for the additive of resol, described method concrete steps are as follows:
(1) cake of camellia oleifera seeds powder is dispersed in water, adds linking agent and stir, obtain mixture a; By mixture a insulation reaction 2~3h at 50~70 DEG C, obtain mixture b;
(2) mixture b is cooled to 30 DEG C, adds curing catalyst and stablizer, stir and insulation reaction 0.5~1h, obtain the additive of resol of the present invention;
A kind of additive application of resol is in phenolic resin adhesive, and phenolic resin adhesive is made up of additive and resol;
Wherein, resol is that solid content is 40~50%, and apparent viscosity is the heat-reactive phenolic resin of 150~1500 centipoises;
Preferably 20~30:100 of the mass ratio of additive and resol.
Beneficial effect
(1) cake of camellia oleifera seeds containing in additive of the present invention belongs to agricultural machining waste, and price is very cheap, can reduce the cost of phenolic resin adhesive; And cake of camellia oleifera seeds contains rich in protein, tannin, tea saponin and robust fibre, these materials solidify time can with resol generation crosslinking reaction, it is the additive that resol is good, can reduce the consumption of traditional resol filler such as flour, soybean protein, effectively reduce the consumption of grain;
(2) curing catalyst and the linking agent that in additive of the present invention, contain, can effectively improve the curing speed of phenolic resin adhesive, shorten the hot pressing time of the wood-based plate of preparation, the methylol of linking agent and amino group can with the active group polymerization reaction take place of resol, and then improve the bonding strength of resin;
(3) in additive of the present invention, contain stablizer, can effectively ensure to add after additive of the present invention phase working life of resol unaffected, make phenolic resin adhesive there is good usability;
(4) preparation method of solidifying agent of the present invention is simple, easy and simple to handle.
Embodiment
With specific embodiment in detail the present invention is described in detail below, but is not limited to this.
In following examples, mentioning resol is heat-reactive phenolic resin, is produced by Tai Er chemical industry (Beijing) company limited, and other main agents information is in table 1; Key instrument and facility information are in table 2;
Table 1
Table 2
Cake of camellia oleifera seeds is residual solid matter after the Extraction oil of seed tea-seed oil of oil tea (Camellia oleifera), and taking cake of camellia oleifera seeds total mass as 100%, camellia seed oil content is 8%, and the granularity of cake of camellia oleifera seeds is 200 orders;
In sodium hydroxide solution, the massfraction of sodium hydroxide is 30%.
Embodiment 1
An additive for resol, taking described additive total mass as 100%, each component and quality percentage composition are as follows:
A preparation method for the additive of resol, described method concrete steps are as follows:
(1) 10kg urea, 13kg formaldehyde and 0.5kg trimeric cyanamide are mixed, add 0.1kg formic acid, stir; Be heated to 85 DEG C, insulation is 12 seconds to being coated with 4 viscosity, is cooled to 70 DEG C, adds 30% sodium hydroxide solution, adjust pH to 7.5, and reaction 15min, is cooled to 30 DEG C, and discharging, obtains cyanurotriamide modified urea resin performed polymer;
(2) 50kg cake of camellia oleifera seeds powder is dispersed in 40kg water, adds 5kg cyanurotriamide modified urea resin performed polymer and stir, obtain mixture a; By mixture a insulation reaction 2h at 50 DEG C, obtain mixture b;
(3) mixture b is cooled to 30 DEG C, adds 4.5kg sodium carbonate and 0.5kg SODIUM PHOSPHATE, MONOBASIC, stir and insulation reaction 1h, obtain the additive of resol.
The key technical indexes of gained resol additive is: solids content is that 56%, pH is 8.2, storage period >=10 day.
(4) the described additive of step (3) and resol are stirred (mass ratio of additive and resol is 30:100), obtain phenolic resin adhesive (being numbered sizing agent 1), wherein resol parameter is: solid content is 40%, and apparent viscosity is 150 centipoises.
Embodiment 2
An additive for resol, taking described additive total mass as 100%, each component and quality percentage composition are as follows:
A preparation method for the additive of resol, described method concrete steps are as follows:
(1) 10kg urea, 13kg formaldehyde and 0.5kg trimeric cyanamide are mixed, add 0.1kg formic acid, stir; Be heated to 85 DEG C, insulation is 15 seconds to being coated with 4 viscosity, is cooled to 70 DEG C, adds 30% sodium hydroxide solution, adjust pH to 7.5, and reaction 15min, is cooled to 30 DEG C, and discharging, obtains cyanurotriamide modified urea resin performed polymer;
(2) 20kg cake of camellia oleifera seeds powder is dispersed in 58kg water, adds 15kg cyanurotriamide modified urea resin performed polymer and stir, obtain mixture a; By mixture a insulation reaction 3h at 70 DEG C, obtain mixture b;
(3) mixture b is cooled to 30 DEG C, adds 5kg glycerol acetate and 2kg borax, stir and insulation reaction 0.5h, obtain the additive of resol.
The key technical indexes of gained resol additive is: solids content is that 35%, pH is 7.8, storage period >=10 day.
(4) the described additive of step (3) and resol are stirred (mass ratio of additive and resol is 20:100), obtain phenolic resin adhesive (being numbered sizing agent 2), wherein resol parameter is: solid content is 50%, and apparent viscosity is 1500 centipoises.
Embodiment 3
An additive for resol, taking described additive total mass as 100%, each component and quality percentage composition are as follows:
A preparation method for the additive of resol, described method concrete steps are as follows:
(1) 10kg urea, 13kg formaldehyde and 0.5kg trimeric cyanamide are mixed, add 0.1kg formic acid, stir; Be heated to 85 DEG C, insulation is 13 seconds to being coated with 4 viscosity, is cooled to 70 DEG C, adds 30% sodium hydroxide solution, adjust pH to 7.5, and reaction 15min, is cooled to 30 DEG C, and discharging, obtains cyanurotriamide modified urea resin performed polymer;
(2) 20kg cake of camellia oleifera seeds powder is dispersed in 70kg water, adds 6kg cyanurotriamide modified urea resin performed polymer and stir, obtain mixture a; By mixture a insulation reaction 2.5h at 60 DEG C, obtain mixture b;
(3) mixture b is cooled to 30 DEG C, adds 3kg propylene carbonate and 1kg Sodium Benzoate, stir and insulation reaction 0.8h, obtain the additive of resol.
The key technical indexes of gained resol additive is: solids content is that 26%, pH is 7.6, storage period >=10 day.
(4) the described additive of step (3) and resol are stirred (mass ratio of additive and resol is 25:100), obtain phenolic resin adhesive (being numbered sizing agent 3), wherein resol parameter is: solid content is 45%, and apparent viscosity is 800 centipoises.
Embodiment 4
An additive for resol, taking described additive total mass as 100%, each component and quality percentage composition are as follows:
A preparation method for the additive of resol, described method concrete steps are as follows:
(1) 10kg urea, 13kg formaldehyde and 0.5kg trimeric cyanamide are mixed, add 0.1kg formic acid, stir; Be heated to 85 DEG C, insulation is 14 seconds to being coated with 4 viscosity, is cooled to 70 DEG C, adds 30% sodium hydroxide solution, adjust pH to 7.5, and reaction 15min, is cooled to 30 DEG C, and discharging, obtains cyanurotriamide modified urea resin performed polymer;
(2) 30kg cake of camellia oleifera seeds powder is dispersed in 55kg water, adds 10kg cyanurotriamide modified urea resin performed polymer and stir, obtain mixture a; By mixture a insulation reaction 3h at 65 DEG C, obtain mixture b;
(3) mixture b is cooled to 30 DEG C, adds 1.5kg propylene carbonate, 2kg sodium carbonate and 1.5kg Sodium phosphate dibasic, stir and insulation reaction 0.6h, obtain the additive of resol.
The key technical indexes of gained resol additive is: solids content is that 43%, pH is 8.0, storage period >=10 day.
(4) the described additive of step (3) and resol are stirred (mass ratio of additive and resol is 25:100), obtain phenolic resin adhesive (being numbered sizing agent 4), wherein resol parameter is: solid content is 48%, and apparent viscosity is 1000 centipoises.
Embodiment 5
An additive for resol, taking described additive total mass as 100%, each component and quality percentage composition are as follows:
A preparation method for the additive of resol, described method concrete steps are as follows:
(1) 10kg urea, 13kg formaldehyde and 0.5kg trimeric cyanamide are mixed, add 0.1kg formic acid, stir; Be heated to 85 DEG C, insulation is 12 seconds to being coated with 4 viscosity, is cooled to 70 DEG C, adds 30% sodium hydroxide solution, adjust pH to 7.5, and reaction 15min, is cooled to 30 DEG C, and discharging, obtains cyanurotriamide modified urea resin performed polymer;
(2) 40kg cake of camellia oleifera seeds powder is dispersed in 45kg water, adds 10kg cyanurotriamide modified urea resin performed polymer and stir, obtain mixture a; By mixture a insulation reaction 2.5h at 70 DEG C, obtain mixture b;
(3) mixture b is cooled to 30 DEG C, adds 3kg sodium carbonate, 1kg borax and 1kg SODIUM PHOSPHATE, MONOBASIC, stir and insulation reaction 1h, obtain the additive of resol.
The key technical indexes of gained resol additive is: solids content is that 48%, pH is 8.4, storage period >=10 day.
(4) the described additive of step (3) and resol are stirred (mass ratio of additive and resol is 23:100), obtain phenolic resin adhesive (being numbered sizing agent 5), wherein resol parameter is: solid content is 45%, and apparent viscosity is 500 centipoises.
Embodiment 6
An additive for resol, taking described additive total mass as 100%, each component and quality percentage composition are as follows:
A preparation method for the additive of resol, described method concrete steps are as follows:
(1) 10kg urea, 13kg formaldehyde and 0.5kg trimeric cyanamide are mixed, add 0.1kg formic acid, stir; Be heated to 85 DEG C, insulation is 12 seconds to being coated with 4 viscosity, is cooled to 70 DEG C, adds 30% sodium hydroxide solution, adjust pH to 7.5, and reaction 15min, is cooled to 30 DEG C, and discharging, obtains cyanurotriamide modified urea resin performed polymer;
(2) 35kg cake of camellia oleifera seeds powder is dispersed in 50kg water, adds 8kg cyanurotriamide modified urea resin performed polymer and stir, obtain mixture a; By mixture a insulation reaction 2h at 60 DEG C, obtain mixture b;
(3) mixture b is cooled to 30 DEG C, adds 3kg sodium carbonate, 2kg glycerol acetate and 1.5kg Sodium Benzoate, 0.5kg borax, stir and insulation reaction 0.5h, obtain the additive of resol.
The key technical indexes of gained resol additive is: solids content is that 42%, pH is 7.8, storage period >=10 day.
(4) the described additive of step (3) and resol are stirred (mass ratio of additive and resol is 20:100), obtain phenolic resin adhesive (being numbered sizing agent 6), wherein resol parameter is: solid content is 45%, and apparent viscosity is 150 centipoises.
Embodiment 7
The effect that utilizes the phenolic resin adhesive of following evidence embodiment 1~6 preparation, particular content is as follows:
With directly additive as a comparison of flour, flour and resol are stirred (mass ratio of flour and resol is 30:100), obtains contrast sizing agent, and wherein resol parameter is: solid content is 40%, and apparent viscosity is 150 centipoises.
Phenolic resin adhesive to embodiment 1~6 preparation and contrast tackiness agent are cured velocity test respectively, working life detects and prepared by 5 layers of poplar plywood.
Wherein, the test of curing speed and working life is carried out according to the corresponding method of detection of regulation in GB/T 14074-2006 " wood adhesive and the resin method of inspection thereof ", and the probe temperature of curing speed is 130 DEG C, and test result is as shown in table 1.
When 5 layers of glued board of preparation, veneer is 5 years quick growth poplar wood veneers (400 millimeters of length, 400 millimeters of width, 1.7 millimeters of thickness), water ratio 12%; The heat pressing process of 5 layers of glued board is: 1.0Mpa, and temperature is 130 DEG C, the time is 5 minutes.
According to the bonding strength of 5 layers of prepared glued board of the tackiness agent of the type Ⅰ plywood bonding strength testing method test implementation example acquisition of regulation in GB/T 17657-1999 " test methods of evaluating the properties of wood-based panels and surface decorated wood-based panels " and contrast tackiness agent, result is as shown in table 1.
Table 1
As seen from Table 1, with phenolic resin adhesive prepared by embodiment of the present invention 1-6 method contrast the curing speed of tackiness agent respectively fast 20.3%, 20.0%, 23.9%, 22.1%, 19.2% and 21.6%; The working life of the phenolic resin adhesive that meanwhile, prepared by embodiment 1-6 method is also long than the working life of contrast tackiness agent.Therefore, the additive of preparing by the inventive method can effectively improve the curing speed of resol, extends the working life of resol.
In addition, be it can also be seen that by table 1, after the additive that adopts the inventive method to prepare mixes with resol, the bonding strength of the phenolic resin adhesive of its acquisition is higher than the bonding strength of the phenolic resin adhesive obtaining using flour as additive, as can be seen here, the additive that prepared by the inventive method can effectively improve the bonding strength of phenolic resin adhesive.
Cost analysis:
At present, phenol price is greatly about 13000 yuan/ton, the cost of the resol of 40% solids content is about 4000 yuan/ton, and cake of camellia oleifera seeds is agricultural machining by product, cheap, price only has 1500 yuan/ton (dry-matteies), and the cost of the resol additive (solids content 56%) of preparing with it is about 1300 yuan/ton; And flour is about 3200 yuan/ton as the market value of additive.Therefore, can calculate the cost of the various phenolic resin adhesives that contain resol additive as shown in table 2.
Table 2
As shown in Table 2, additive of the present invention joins after resol, can significantly lower the cost value of phenolic resin adhesive, and compared with the additive flour conventional with resol, its price advantage is obvious.
The present invention includes but be not limited to above embodiment, every any being equal to of carrying out under the principle of spirit of the present invention, replaces or local improvement, all will be considered as within protection scope of the present invention.

Claims (7)

1. an additive for resol, is characterized in that: taking described additive total mass as 100%, each component and quality percentage composition are as follows:
2. the additive of a kind of resol according to claim 1, it is characterized in that: residual solid matter after the Extraction oil of seed tea-seed oil that described cake of camellia oleifera seeds is oil tea, taking cake of camellia oleifera seeds total mass as 100%, wherein, camellia seed oil content is less than 10%, and the granularity of cake of camellia oleifera seeds is less than or equal to 200 orders.
3. the additive of a kind of resol according to claim 1, is characterized in that: described linking agent is cyanurotriamide modified urea resin performed polymer.
4. the additive of a kind of resol according to claim 3, is characterized in that: the preparation method of described cyanurotriamide modified urea resin performed polymer is as follows:
Urea, formaldehyde and trimeric cyanamide are mixed, add formic acid, stir; Be heated to 85 DEG C, insulation is 12~15 seconds to being coated with 4 viscosity, is cooled to 70 DEG C, adds sodium hydroxide solution, adjust pH to 7.5, and reaction 15min, is cooled to 30 DEG C, and discharging, obtains described cyanurotriamide modified urea resin performed polymer;
Wherein, the mass ratio of described urea, formaldehyde, trimeric cyanamide and formic acid is 1:1.3:0.05:0.01;
In sodium hydroxide solution, the massfraction of sodium hydroxide is 30%.
5. the additive of a kind of resol according to claim 1, is characterized in that: described curing catalyst is more than one in sodium carbonate, glycerol acetate and propylene carbonate; Stablizer is more than one in SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate dibasic, borax and Sodium Benzoate.
6. a preparation method for the additive of resol as claimed in claim 1, is characterized in that: described method steps is as follows:
(1) cake of camellia oleifera seeds powder is dispersed in water, adds linking agent and stir, obtain mixture a; By mixture a insulation reaction 2~3h at 50~70 DEG C, obtain mixture b;
(2) mixture b is cooled to 30 DEG C, adds curing catalyst and stablizer, stir and insulation reaction 0.5~1h, obtain the additive of described resol.
7. the application of the additive of a resol as claimed in claim 1, it is characterized in that: described additive is for phenolic resin adhesive, phenolic resin adhesive is made up of additive and resol, wherein, resol is that solid content is 40~50%, and apparent viscosity is the heat-reactive phenolic resin of 150~1500 centipoises; The mass ratio of additive and resol is 20~30:100.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104944882A (en) * 2015-06-19 2015-09-30 盐城工学院 High-strength water-resistant type desulfurized gypsum board and preparation method thereof
CN107057667A (en) * 2017-04-28 2017-08-18 中国石油天然气集团公司 A kind of modified phenolic crosslinking agent and its preparation method and application
CN109705781A (en) * 2018-12-29 2019-05-03 广西六万山林业有限公司 A kind of Enviorment-protective Phenolic Resin glue and the preparation method and application thereof
CN111154437A (en) * 2019-12-25 2020-05-15 上海昶法新材料有限公司 Phenolic resin additive and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101580684A (en) * 2009-06-05 2009-11-18 烟台德邦科技有限公司 Low-temperature fast curing underfill adhesive and preparation method thereof
CN103304956A (en) * 2013-07-11 2013-09-18 常熟市慧丰塑料制品有限公司 Formula of modified phenolic resin

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101580684A (en) * 2009-06-05 2009-11-18 烟台德邦科技有限公司 Low-temperature fast curing underfill adhesive and preparation method thereof
CN103304956A (en) * 2013-07-11 2013-09-18 常熟市慧丰塑料制品有限公司 Formula of modified phenolic resin

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104944882A (en) * 2015-06-19 2015-09-30 盐城工学院 High-strength water-resistant type desulfurized gypsum board and preparation method thereof
CN104944882B (en) * 2015-06-19 2017-01-18 盐城工学院 High-strength water-resistant type desulfurized gypsum board and preparation method thereof
CN107057667A (en) * 2017-04-28 2017-08-18 中国石油天然气集团公司 A kind of modified phenolic crosslinking agent and its preparation method and application
CN107057667B (en) * 2017-04-28 2020-04-21 中国石油天然气集团公司 Modified phenolic crosslinking agent and preparation method and application thereof
CN109705781A (en) * 2018-12-29 2019-05-03 广西六万山林业有限公司 A kind of Enviorment-protective Phenolic Resin glue and the preparation method and application thereof
CN111154437A (en) * 2019-12-25 2020-05-15 上海昶法新材料有限公司 Phenolic resin additive and preparation method thereof

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