CN102268130A - Preparation method of biochemical polyol - Google Patents
Preparation method of biochemical polyol Download PDFInfo
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- CN102268130A CN102268130A CN 201110163929 CN201110163929A CN102268130A CN 102268130 A CN102268130 A CN 102268130A CN 201110163929 CN201110163929 CN 201110163929 CN 201110163929 A CN201110163929 A CN 201110163929A CN 102268130 A CN102268130 A CN 102268130A
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Abstract
The invention discloses a preparation method of a biochemical polyol, and the process comprises the following steps: adding raffinate or residues of waste dicarboxylic acids and diol residues into a reaction vessel, slowly heating to 180 DEG C-246 DEG C, stirring continuously, performing heat insulation for 20-30 hours, cooling to below 100 DEG C to form a homogenous body, adding ammonia gas to allow the pressure in the vessel to become an atmospheric pressure, realizing esterification, cracking, transesterification, and polymerization during heating so as to form a homogenous body. The method produces the biochemical polyol by using waste materials such as alcohol residues and acid residues which can cause pollution to water and soil resources, and the biochemical polyol produced by the method is stable, has extensive raw material sources and low cost, can change waste into valuables, solves the problem of environmental pollution, and realizes energy substitution and reutilization.
Description
Technical field
The invention belongs to the petrochemical technology field, be specifically related to a kind of preparation method who utilizes pure slag, acid sludge waste material and useless PET, the biochemical polyvalent alcohol of PED material produce
Background technology
Urethane extensively applies to all trades and professions of national defence, communications and transportation and national economy.Can be used as sandwich sheet material, building wall, house component aspect building, the effect with sound-absorbing, thermal insulation, thermal insulation, antiseep can be used as the heat-insulation and heat-preservation material of oil depot, oil tank, petroleum pipe line, chemical plant conversion unit; Militarily can be used as the ablative-insulative material of spaceship shell, the packing material of aircraft wing, tail, guided missile rocket external fairings etc.Along with the fast development of Chinese national economy, the demand of polyurethane products is also being increased sharply.All polyurethane products all are from the oil deep processing, but utilize oil production urethane that himself limitation and drawback are arranged.At first be to have wasted a large amount of petroleum resources, China is an energy demand big country, especially oil, exist very big gap between oil reserves of China and the demand, next is that the environmental pollution that utilizes oil production urethane to cause is very serious, huge and lasting to environment damage power, up to now, worldwide still there is not good solution.Therefore and biochemical polyol resin is one of important source material of synthesis of polyurethane, seeks a kind of alternative materials, and not relying on oil is the problem that the technician is exploring always as the method for the biochemical polyol resin of raw material production.
Summary of the invention
The purpose of this invention is to provide a kind of utilization water and soil resources are produced pure slag, acid sludge waste material and the useless PET that pollutes, the preparation method of the biochemical polyvalent alcohol of PED material produce, the biochemical polyvalent alcohol stability that this method is produced, raw material sources are extensive, cost is low, turn waste into wealth, solved environmental pollution and also realized substituting and utilizing again of the energy.
For achieving the above object, the technical solution used in the present invention is: the preparation method of this biochemistry polyvalent alcohol is characterized in that according to following step preparation:
Get 600 parts of the raffinate of useless diprotic acid or residues by weight, get 400 parts of dibasic alcohol residues again, to slowly be heated to 180 ℃～246 ℃ and continuously stirring in above-mentioned diprotic acid and the dibasic alcohol material adding reactor, be incubated 20-30 hour, be cooled to and become equal one below 100 ℃, add ammonia, the still internal pressure is a normal atmosphere, discharging.
The optimum heating temperature of optimizing is controlled at 210 ℃～230 ℃.
Adopt above-mentioned preparation method's beneficial effect: the flow process of this method is batching, fatization, cracking, transesterify, polymerization, be from the residue waste liquid of petrochemical industry byproduct, to extract biochemical polyol resin, can well solve China's chemistry polyvalent alcohol, the polyprotonic acid waste liquid, the environmental pollution that cause in this field of waste residue, turn waste into wealth, realize the utilization again of the energy, the utilization ratio of residue waste liquid reaches 95～98%, and produce in the process of chemical polyvalent alcohol utilizing the residue waste liquid, do not produce any waste gas, waste liquid, waste residue, can not produce secondary pollution, production process realizes zero release substantially.This product is measured through Henan Province inspection center, the biochemical polyol resin synthetic resistant polyurethane thermostability that this method is produced is more than 184 ℃, thermal conductivity is 0.016～0.02, temperature tolerance exceeds 84 ℃ of urethane on the market, deformation is lower than 1/1000, as basic trimerization is poly-isocyanurate, and then performance is more superior, becomes good heat insulating energy saving material.The biochemical polyvalent alcohol of the present invention preparation is after tested: hydroxyl value 450, viscosity 1500, acid number 0.7-1.5.By anti-500 ℃ of compound insulating materials that the patented product is made, Nikkei Henan Prov. Analytical Test Center tested December 18 in 2000, thermal resistance (m
2.K/W) 0.985; Heatproof test: 184.2 ℃ of organic layer heat decomposition temperatures, 92.7 ℃ of interface equilibrium temperatures, (no machine side is heated 500 ℃, 2h), high temperature resistantly exceeds 84 ℃ of like products, and performance has met or exceeded main polyester polyol abroad.Parameter as the external polyester polyol of following table:
Embodiment
The preparation method of this biochemistry polyvalent alcohol prepares according to following step:
Get 600 parts of the raffinate of useless diprotic acid or residues by weight, get 400 parts of dibasic alcohol residues again, to slowly be heated to 180 ℃～246 ℃ and continuously stirring in above-mentioned diprotic acid and the dibasic alcohol material adding reactor, be incubated 20-30 hour, be cooled to and become equal one below 100 ℃, add ammonia, the still internal pressure is a normal atmosphere, discharging.
Main consideration fatization and transesterification reaction among this preparation method, because the composition of glycol and boiling point are not quite identical, its boiling point is between 160 ℃～280 ℃, and temperature of reaction is higher than or near boiling point, then loss of material is more, reaction is incomplete, and the reaction product alcohols is very few, and temperature is on the low side, reaction temperature is spent slowly, reaction times is long, so temperature of reaction is controlled at 180 ℃～246 ℃, and Best Times is controlled at 210 ℃～230 ℃.The raffinate of the useless binary in the inventive method or residue, dibasic alcohol residue consumption should can change about 5% to any direction according to finish mix viscosity, hydroxyl value and acidity with mol ratio as foundation.From the reason human relations, in the depolymerization reaction process, a structural unit needs 1mol alcohol, and in the transesterify process, a structural unit needs 2mol alcohol.Therefore, the molar ratio of useless diprotic acid residue and dibasic alcohol residue is a main operating parameters, should be 1-2,, obtain mol ratio and polyester hydroxyl value and viscosity relationship by different mole preparation polyester polyols, increase along with mol ratio, the polyester viscosity degradation, when mol ratio greater than 1.2 the time, viscosity changes and eases up, consider the flowability of material, selection viscosity is 200-4000mpa.s.
Biochemical polyvalent alcohol is used: 1, get biochemical polyvalent alcohol 100 grams, tensio-active agent 1.5～3 grams, catalyzer 2～3 grams, CFC141b 30～40 grams in 20 ℃～25 ℃ temperature, stirred 4 hours with 1400 rev/mins electric blender; 2, get MDI 50 gram and be placed in the enamelled vessel (1000ml), get combination material 50 grams again, two kinds of material back of putting together was stirred 20～30 seconds, can rise and send out a synthetic required rigid urethane foam, density is about 45Kg/m
3About, also can adjust the density size according to customer need.
Claims (2)
1. the preparation method of a biochemical polyvalent alcohol is characterized in that according to following step preparation:
Get 600 parts of the raffinate of useless diprotic acid or residues by weight, get 400 parts of dibasic alcohol residues again, to slowly be heated to 180 ℃～246 ℃ and continuously stirring in above-mentioned diprotic acid and the dibasic alcohol material adding reactor, be incubated 20-30 hour, be cooled to and become equal one below 100 ℃, add ammonia, the still internal pressure is a normal atmosphere, discharging.
2. the preparation method of biochemical polyvalent alcohol according to claim 1, it is characterized in that: heating and temperature control is at 210 ℃～230 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110163929 CN102268130A (en) | 2011-06-17 | 2011-06-17 | Preparation method of biochemical polyol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110163929 CN102268130A (en) | 2011-06-17 | 2011-06-17 | Preparation method of biochemical polyol |
Publications (1)
| Publication Number | Publication Date |
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| CN102268130A true CN102268130A (en) | 2011-12-07 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 201110163929 Pending CN102268130A (en) | 2011-06-17 | 2011-06-17 | Preparation method of biochemical polyol |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1487001A (en) * | 2003-08-07 | 2004-04-07 | 烟台万华聚氨酯股份有限公司 | Production process and use of polyester polyol and its modifying material |
| CN101029124A (en) * | 2007-04-10 | 2007-09-05 | 中国林业科学研究院林产化学工业研究所 | Rosin polyester polyhydric-alcohol for hard polyurethane foaming plastic and its production |
| CN101265323A (en) * | 2007-03-16 | 2008-09-17 | 张鹏飞 | Polyester polyol |
| WO2010142399A1 (en) * | 2009-06-10 | 2010-12-16 | Bayer Materialscience Ag | Process for producing polyester polyols with low quantities of dioxan waste |
-
2011
- 2011-06-17 CN CN 201110163929 patent/CN102268130A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1487001A (en) * | 2003-08-07 | 2004-04-07 | 烟台万华聚氨酯股份有限公司 | Production process and use of polyester polyol and its modifying material |
| CN101265323A (en) * | 2007-03-16 | 2008-09-17 | 张鹏飞 | Polyester polyol |
| CN101029124A (en) * | 2007-04-10 | 2007-09-05 | 中国林业科学研究院林产化学工业研究所 | Rosin polyester polyhydric-alcohol for hard polyurethane foaming plastic and its production |
| WO2010142399A1 (en) * | 2009-06-10 | 2010-12-16 | Bayer Materialscience Ag | Process for producing polyester polyols with low quantities of dioxan waste |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20111207 |