CN103865017A - Environment-friendly phenolic resin preparation process without wastewater discharge - Google Patents
Environment-friendly phenolic resin preparation process without wastewater discharge Download PDFInfo
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- CN103865017A CN103865017A CN201410113141.4A CN201410113141A CN103865017A CN 103865017 A CN103865017 A CN 103865017A CN 201410113141 A CN201410113141 A CN 201410113141A CN 103865017 A CN103865017 A CN 103865017A
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- Prior art keywords
- paraformaldehyde
- catalyzer
- composition
- resol
- preparation process
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000002351 wastewater Substances 0.000 title claims abstract description 28
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 title abstract description 5
- 229920001568 phenolic resin Polymers 0.000 title abstract description 5
- 239000005011 phenolic resin Substances 0.000 title abstract description 5
- 229930040373 Paraformaldehyde Natural products 0.000 claims abstract description 59
- 229920002866 paraformaldehyde Polymers 0.000 claims abstract description 59
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 229920003987 resole Polymers 0.000 claims description 44
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 16
- -1 compound rare-earth Chemical group 0.000 claims description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 229910052684 Cerium Inorganic materials 0.000 claims description 8
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 8
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 8
- 229910052779 Neodymium Inorganic materials 0.000 claims description 8
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 8
- 229910052772 Samarium Inorganic materials 0.000 claims description 8
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims description 8
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims description 8
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 8
- 229910052746 lanthanum Inorganic materials 0.000 claims description 8
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 8
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 8
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims description 8
- 229910052706 scandium Inorganic materials 0.000 claims description 8
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 8
- 229910052727 yttrium Inorganic materials 0.000 claims description 8
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 239000000470 constituent Substances 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 26
- 238000000034 method Methods 0.000 abstract description 8
- 239000007788 liquid Substances 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract 4
- 238000007599 discharging Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 230000035484 reaction time Effects 0.000 abstract 1
- 229920001187 thermosetting polymer Polymers 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 206010000372 Accident at work Diseases 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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Abstract
The invention relates to an environment-friendly phenolic resin preparation process without wastewater discharge. The process comprises the following steps: firstly, adding molten phenol into a reactor; then heating to 50 DEG C to 90 DEG C; starting and continuously adding paraformaldehyde and a catalyst for 2 to 5 hours and controlling heat release during a reaction according to the adding rate of the paraformaldehyde and the catalyst; further reacting in a heat preservation manner until the desired viscosity of materials is achieved after the adding of the paraformaldehyde and the catalyst; and then cooling and discharging, thereby obtaining a phenolic resin product. The thermosetting phenolic resin is prepared by replacing the existing liquid formaldehyde with the paraformaldehyde; the smooth reaction of the paraformaldehyde and the phenol is realized by controlling the adding mode of the paraformaldehyde and the catalyst as well as the reaction temperature and the reaction time, so that the difficult problem that the heat release during the high-concentration reaction of the paraformaldehyde and the phenol is too drastic so as to be difficult to control is solved.
Description
Technical field
The present invention relates to a kind of preparation technology of resol, specifically a kind of resol green preparation process that adopts paraformaldehyde raw material non-wastewater discharge.
Background technology
Resol is widely used in the fields such as building, traffic, aerospace as a kind of industry adhesive, but the preparation of resol at present adopts phenol and liquid formaldehyde (37% formalin) react and make more.Owing to containing a large amount of water in reaction raw materials, inevitably produce a large amount of waste water preparing in resol process, resol per ton approximately produces the waste water of 500-700Kg.These waste water have caused very large difficulty to follow-up waste water treatment, have become the bottleneck problem of restriction resol industry development.
Adopt paraformaldehyde (solid formaldehyde) to substitute liquid formaldehyde and prepare the preparation technology that resol is a kind of advanced person, because reaction former material (formaldehyde) purity is high, therefore prepare resol and substantially do not produce waste water, therefore adopting paraformaldehyde to prepare resol is the effective way that solution resol industry causes environmental pollution.But due to the reacting of paraformaldehyde and phenol, because reaction product concentration is high, exothermic heat of reaction is violent,, causes casualties and property damage often because exothermic heat of reaction acutely causes implode, the industrial accidents such as still of overflowing for large-scale batch preparation on the other hand.Therefore how realizing paraformaldehyde, to prepare the controllable reaction of resol be technical barrier prepared by resol greenization.
Summary of the invention
Technical problem to be solved by this invention is:
How to solve the too fierce unmanageable technical problem of high density exothermic heat of reaction of paraformaldehyde and phenol;
The technical scheme that the present invention solves above technical problem is:
A kind of resol green preparation process of non-wastewater discharge, in reactor, first add the phenol of melting, then be warmed up to 50-90 DEG C, then divide 2-6 time and on average paraformaldehyde and catalyzer be dosed in reactor with screw rod boost pump, paraformaldehyde and catalyzer added in 2-5 hour, after paraformaldehyde and catalyzer add, continued insulation and reacted at 75～85 DEG C the viscosity that reaches expection to material, then cooling discharge, obtains resol product.
Like this, the present invention adds technique continuously by paraformaldehyde and catalyzer, solves current paraformaldehyde and prepares in resol process and exist reaction to be acutely difficult to stable control, is unfavorable for a difficult problem for suitability for industrialized production.
The technical scheme that the present invention further limits is:
The resol green preparation process of aforesaid non-wastewater discharge, the mol ratio of wherein said paraformaldehyde and phenol is 0.5～2.0:2.0～0.5; The mol ratio of described catalyzer and phenol is 0.1%～0.5%.
The resol green preparation process of aforesaid non-wastewater discharge, wherein catalyzer is at least one in sodium hydroxide, potassium hydroxide, hydrated barta, ammoniacal liquor and sodium carbonate.
The resol green preparation process of aforesaid non-wastewater discharge, the composition A that wherein catalyzer is 99.1-99.3% by weight percent and the composition B of 0.7-0.9% form; Composition A is at least one mixing in sodium hydroxide, potassium hydroxide, hydrated barta, ammoniacal liquor and sodium carbonate; Composition B is compound rare-earth; The weight percent component of compound rare-earth is: lanthanum: 12-15%, cerium: 15-18%, scandium: 16-19%, yttrium: 9-11%, samarium: 7-9%, neodymium: 11-13%, gadolinium: 7-9%, praseodymium: 1-3%, dysprosium: 8-15%, all the other lanthanon: 1-3%, the component sum of above each rare earth element is 100%; In catalyzer, by adding compound rare-earth, only need divide and also on average paraformaldehyde and catalyzer are dosed in reactor for 2 to 3 times with screw rod boost pump, paraformaldehyde and catalyzer can add in 2-3 hour; Both solve current paraformaldehyde and prepared the technical problem that in resol process, existence reaction is acutely difficult to stable control, and reduced again and added indegree, and improved speed of response, killed two birds with one stone, played beyond thought technique effect.
The present invention adopts the alternative existing liquid formaldehyde of paraformaldehyde to prepare heat-reactive phenolic resin, by paraformaldehyde and catalyzer added to mode and the control of temperature of reaction and time, realize the smooth reaction of paraformaldehyde and phenol, solve the too fierce unmanageable difficult problem of high density exothermic heat of reaction of paraformaldehyde and phenol; Preparation method of the present invention has that technique is simple, operational safety, be easy to the feature of large-scale mass production.
Formaldehyde of the present invention is paraformaldehyde, thereby has avoided large water gaging in traditional liquid formaldehyde to have the wastewater problem bringing; In the present invention, adopted the technique that adds continuously of paraformaldehyde and catalyzer to control exothermic heat of reaction, realizing paraformaldehyde, to prepare the reaction of resol controlled.
Embodiment
embodiment 1
The present embodiment is a kind of resol green preparation process of non-wastewater discharge, in reactor, first add the phenol of melting, then be warmed up to 50 DEG C, then divide 4 times and on average paraformaldehyde and catalyzer be dosed in reactor with screw rod boost pump, paraformaldehyde and catalyzer added in 4 hours, after paraformaldehyde and catalyzer add, continued insulation and reacted at 75 DEG C the viscosity that reaches expection to material, then cooling discharge, obtains resol product.
Wherein the mol ratio of paraformaldehyde and phenol is 0.5:2.0; The mol ratio of catalyzer and phenol is 0.1%; Wherein catalyzer is sodium hydroxide.
embodiment 2
The present embodiment is a kind of resol green preparation process of non-wastewater discharge, in reactor, first add the phenol of melting, then be warmed up to 70 DEG C, then divide 5 times and on average paraformaldehyde and catalyzer be dosed in reactor with screw rod boost pump, paraformaldehyde and catalyzer added in 5 hours, after paraformaldehyde and catalyzer add, continued insulation and reacted at 80 DEG C the viscosity that reaches expection to material, then cooling discharge, obtains resol product.
Wherein the mol ratio of paraformaldehyde and phenol is 1.0:1.0; The mol ratio of catalyzer and phenol is 0.3%.Wherein catalyzer is potassium hydroxide.
embodiment 3
The present embodiment is a kind of resol green preparation process of non-wastewater discharge, in reactor, first add the phenol of melting, then be warmed up to 90 DEG C, then divide 6 times and on average paraformaldehyde and catalyzer be dosed in reactor with screw rod boost pump, paraformaldehyde and catalyzer added in 3 hours, after paraformaldehyde and catalyzer add, continued insulation and reacted at 85 DEG C the viscosity that reaches expection to material, then cooling discharge, obtains resol product.
Wherein the mol ratio of paraformaldehyde and phenol is 2.0:0.5; The mol ratio of catalyzer and phenol is 0.5%.Wherein catalyzer is the mixing in ammoniacal liquor and sodium carbonate.
embodiment 4
The present embodiment is a kind of resol green preparation process of non-wastewater discharge, in reactor, first add the phenol of melting, then be warmed up to 50 DEG C, then divide 2 times and on average paraformaldehyde and catalyzer be dosed in reactor with screw rod boost pump, paraformaldehyde and catalyzer added in 2 hours, after paraformaldehyde and catalyzer add, continued insulation and reacted at 75 DEG C the viscosity that reaches expection to material, then cooling discharge, obtains resol product.
Wherein the mol ratio of paraformaldehyde and phenol is 1.5:2.0; The mol ratio of catalyzer and phenol is 0.3%.The composition A that catalyzer is 99.1% by weight percent and 0.9% composition B form; Composition A is sodium hydroxide; Composition B is compound rare-earth; The constituent mass per-cent of compound rare-earth is: lanthanum: 12%, and cerium: 18%, scandium: 19%, yttrium: 9%, samarium: 7%, neodymium: 11%, gadolinium: 7%, praseodymium: 1%, dysprosium: 15%, all the other lanthanon: 1%.
embodiment 5
The present embodiment is a kind of resol green preparation process of non-wastewater discharge, the present embodiment is a kind of resol green preparation process of non-wastewater discharge, in reactor, first add the phenol of melting, then be warmed up to 80 DEG C, then divide 3 times and on average paraformaldehyde and catalyzer be dosed in reactor with screw rod boost pump, paraformaldehyde and catalyzer added in 3 hours, after paraformaldehyde and catalyzer add, continue insulation and react at 80 DEG C the viscosity that reaches expection to material, then cooling discharge, obtains resol product.
Wherein the mol ratio of paraformaldehyde and phenol is 1..0:0.5; The mol ratio of catalyzer and phenol is 0.2%.The composition A that catalyzer is 99.2% by weight percent and 0.8% composition B form; Composition A is potassium hydroxide; The constituent mass per-cent of compound rare-earth is: lanthanum: 15%, and cerium: 15%, scandium: 16%, yttrium: 11%, samarium: 8%, neodymium: 13%, gadolinium: 8%, praseodymium: 2%, dysprosium: 10%, all the other lanthanon: 2%.
embodiment 6
The present embodiment is a kind of resol green preparation process of non-wastewater discharge, the present embodiment is a kind of resol green preparation process of non-wastewater discharge, in reactor, first add the phenol of melting, then be warmed up to 90 DEG C, then divide 3 times and on average paraformaldehyde and catalyzer be dosed in reactor with screw rod boost pump, paraformaldehyde and catalyzer added in 3 hours, after paraformaldehyde and catalyzer add, continue insulation and react at 85 DEG C the viscosity that reaches expection to material, then cooling discharge, obtains resol product.
Wherein the mol ratio of paraformaldehyde and phenol is 1.8:0.8; The mol ratio of catalyzer and phenol is 0.4%.The composition A that catalyzer is 99.3% by weight percent and 0.7% composition B form; Composition A is ammoniacal liquor; The constituent mass per-cent of compound rare-earth is: lanthanum: 13%, and cerium: 16%, scandium: 17%, yttrium: 10%, samarium: 9%, neodymium: 12%, gadolinium: 9%, praseodymium: 3%, dysprosium: 8%, all the other lanthanon: 3%.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.
Claims (7)
1. the resol green preparation process of a non-wastewater discharge, it is characterized in that: the phenol that first adds melting in reactor, then be warmed up to 50-90 DEG C, then divide 2-6 time and on average paraformaldehyde and catalyzer be dosed in reactor with screw rod boost pump, paraformaldehyde and catalyzer added in 2-5 hour, after paraformaldehyde and catalyzer add, continued insulation and reacted at 75～85 DEG C the viscosity that reaches expection to material, then cooling discharge, obtains resol product.
2. the resol green preparation process of non-wastewater discharge as claimed in claim 1, is characterized in that: the mol ratio of described paraformaldehyde and phenol is 0.5～2.0:2.0～0.5; The mol ratio of described catalyzer and phenol is 0.1%～0.5%.
3. the resol green preparation process of non-wastewater discharge as claimed in claim 1 or 2, is characterized in that: described catalyzer is at least one in sodium hydroxide, potassium hydroxide, hydrated barta, ammoniacal liquor and sodium carbonate.
4. the resol green preparation process of non-wastewater discharge as claimed in claim 1 or 2, is characterized in that: the composition A that described catalyzer is 99.1-99.3% by weight percent and the composition B of 0.7-0.9% form; Described composition A is at least one mixing in sodium hydroxide, potassium hydroxide, hydrated barta, ammoniacal liquor and sodium carbonate; Described composition B is compound rare-earth; The weight percent component of described compound rare-earth is: lanthanum: 12-15%, cerium: 15-18%, scandium: 16-19%, yttrium: 9-11%, samarium: 7-9%, neodymium: 11-13%, gadolinium: 7-9%, praseodymium: 1-3%, dysprosium: 8-15%, all the other lanthanon: 1-3%, the component sum of above each rare earth element is 100%; In catalyzer, by adding compound rare-earth, divide and also on average paraformaldehyde and catalyzer are dosed in reactor for 2-3 time with screw rod boost pump, paraformaldehyde and catalyzer added in 2-3 hour.
5. the resol green preparation process of non-wastewater discharge as claimed in claim 4, is characterized in that: the composition A that described catalyzer is 99.1% by weight percent and 0.9% composition B form; Described composition A is sodium hydroxide; Described composition B is compound rare-earth; The constituent mass per-cent of described compound rare-earth is: lanthanum: 12%, and cerium: 18%, scandium: 19%, yttrium: 9%, samarium: 7%, neodymium: 11%, gadolinium: 7%, praseodymium: 1%, dysprosium: 15%, all the other lanthanon: 1%.
6. the resol green preparation process of non-wastewater discharge as claimed in claim 4, is characterized in that: the composition A that described catalyzer is 99.2% by weight percent and 0.8% composition B form; Described composition A is potassium hydroxide; The constituent mass per-cent of described compound rare-earth is: lanthanum: 15%, and cerium: 15%, scandium: 16%, yttrium: 11%, samarium: 8%, neodymium: 13%, gadolinium: 8%, praseodymium: 2%, dysprosium: 10%, all the other lanthanon: 2%.
7. the resol green preparation process of non-wastewater discharge as claimed in claim 4, is characterized in that: the composition A that described catalyzer is 99.3% by weight percent and 0.7% composition B form; Described composition A is ammoniacal liquor; The constituent mass per-cent of described compound rare-earth is: lanthanum: 13%, and cerium: 16%, scandium: 17%, yttrium: 10%, samarium: 9%, neodymium: 12%, gadolinium: 9%, praseodymium: 3%, dysprosium: 8%, all the other lanthanon: 3%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410113141.4A CN103865017B (en) | 2014-03-25 | 2014-03-25 | A kind of resol green preparation process of non-wastewater discharge |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410113141.4A CN103865017B (en) | 2014-03-25 | 2014-03-25 | A kind of resol green preparation process of non-wastewater discharge |
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| CN103865017A true CN103865017A (en) | 2014-06-18 |
| CN103865017B CN103865017B (en) | 2015-08-19 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1566172A (en) * | 2003-06-27 | 2005-01-19 | 上海尖端工程材料有限公司 | Foam type phenol-formaldehyde resin and its production technology |
| CN102086256A (en) * | 2010-12-28 | 2011-06-08 | 何洪清 | Method for synthesizing high-performance non-dehydration foamed phenolic resin |
| CN102443126A (en) * | 2011-09-02 | 2012-05-09 | 王博 | Low-temperature foaming phenolic resin, preparation method thereof and preparation method of modified phenolic foam |
| CN102850496A (en) * | 2012-03-21 | 2013-01-02 | 山东圣泉化工股份有限公司 | High-ortho phenolic resin and preparation method thereof |
-
2014
- 2014-03-25 CN CN201410113141.4A patent/CN103865017B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1566172A (en) * | 2003-06-27 | 2005-01-19 | 上海尖端工程材料有限公司 | Foam type phenol-formaldehyde resin and its production technology |
| CN102086256A (en) * | 2010-12-28 | 2011-06-08 | 何洪清 | Method for synthesizing high-performance non-dehydration foamed phenolic resin |
| CN102443126A (en) * | 2011-09-02 | 2012-05-09 | 王博 | Low-temperature foaming phenolic resin, preparation method thereof and preparation method of modified phenolic foam |
| CN102850496A (en) * | 2012-03-21 | 2013-01-02 | 山东圣泉化工股份有限公司 | High-ortho phenolic resin and preparation method thereof |
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