Synthesis method of polyester polyol

A technology of polyester polyol and synthesis device, which is applied in the synthesis field of polyester polyol, can solve the problems of high COD of small molecular polyol, loss of small molecular polyol, slow reaction speed of materials, etc. The effect of short time and fast response

Active Publication Date: 2015-07-01
梅法洪
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] 2. Lose a certain amount of small molecule polyols
Even if the top temperature of the reflux condenser B1 can be precisely controlled at 100-105°C, a certain amount of small molecule polyols will still be entrained by water vapor, so the excess of small molecule polyols is about 5% higher than the theoretical value
[0016] 3. High energy consumption
resulting in high energy consumption in the entire reaction process
[0017] 4. Long response time
During the reaction process, the condensed water is continuously refluxed and cannot be discharged in time, which inhibits the reaction, and there is water, the temperature of the material rises slowly, the reaction speed of the material is slow, and the reaction time is prolonged
[0018] 5. High cost of wastewater treatment
However, due to the high COD of small molecule polyols entrained by water vapor, the cost of wastewater treatment is high
[0019] At present, some more advanced devices are figure 2 The reflux condenser B1 is changed to a distillation column, which can effectively reduce the discharge of small molecular polyols with water vapor, but it also has problems such as long reaction time and high energy consumption.

Method used

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  • Synthesis method of polyester polyol
  • Synthesis method of polyester polyol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The production device of this embodiment is as simple as figure 1 As shown, the stainless steel jacketed reactor A2 has a volume of 6000L, the 2 square meter shell and tube stainless steel reflux condenser B2, the 4000L stainless steel intermediate tank C, and the intermediate tank C is equipped with 4000kg Molecular sieve, W-4 reciprocating vacuum system (including water collection tank), 260 degree hot oil, nitrogen.

[0046]Put 3212kg of adipic acid and 1488kg of ethylene glycol into the reaction kettle, heat up, the temperature of the material rises to 100°C, start stirring, turn on the cooling water of the reflux condenser B2, control the top temperature of the reflux condenser B2 to 90°C, and when the temperature of the material rises to 210 ℃, the top temperature of the reflux condenser B2 is turned off and the cooling water drops to 60℃, and the vacuum is turned on. Before turning on the vacuum, the cooling water of the reflux condenser B2 should be turned on ...

Embodiment 2

[0049] In the reaction device of embodiment 1, drop into 2628kg adipic acid, 2120kg diethylene glycol, heat up, material temperature rises to 100 ℃ and stir, open reflux condenser B2 cooling water, control reflux condenser B2 top temperature 90 ℃, when When the temperature of the material rises to 210°C, turn off the cooling water in the reflux condenser B2 and turn on the vacuum when the top temperature drops to 60°C. Before turning on the vacuum, turn on the cooling water of the reflux condenser B2 again, and control the top temperature of the reflux condenser B2 to 65°C. The vacuum degree of the system starts from -0.02MPa, and the vacuum degree increases every half an hour, in order of -0.04MPa, -0.06MPa, -0.08MPa, -0.095MPa. Then react under vacuum for another 4.5 hours. Sampling, acid value 1.85mgKOH / g.

[0050] The total reaction time is about 16 hours. The molecular weight of polyester polyol is 2040.

Embodiment 3

[0052] In the reaction device of embodiment 1, drop into 3182.8kg adipic acid, 1339.2kg ethylene glycol, 198kg trimethylolpropane, heat up, the material temperature rises to 100 ℃ and start stirring, open reflux condenser B2 cooling water, control reflux condensation The top temperature of the condenser B2 is 90°C. When the material temperature rises to 210°C, turn off the cooling water in the reflux condenser B2 and the top temperature drops to 60°C, and turn on the vacuum. Before turning on the vacuum, turn on the cooling water of the reflux condenser B2 again to control the reflux condensation The top temperature of vessel B2 is 65°C, the vacuum degree of the reaction system starts from -0.02MPa, and the vacuum degree increases every half an hour, in order of -0.04MPa, -0.06MPa, -0.08MPa, -0.095MPa. Then react under vacuum for another 4.5 hours. Sampling, acid value 1.81mgKOH / g.

[0053] The total reaction time is about 16 hours. The molecular weight of polyester polyol i...

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Abstract

The invention discloses a synthesis device of polyester polyol. The synthesis device comprises a reaction kettle, a reflux condenser, an intermediate tank and a second condenser, wherein the reaction kettle is provided with a heat conduction oil inlet and a heat conduction oil outlet; the reflux condenser is provided with a coolant inlet and a coolant outlet; the second condenser is provided with the coolant inlet and the coolant outlet; the reaction kettle is communicated with the intermediate tank, the intermediate tank is communicated with the reflux condenser; the intermediate tank is filled with a water-absorbing substance; the outlet of the reflux condenser is provided with a temperature control point; the reflux condenser is communicated with the second condenser, the reaction outlet of the second condenser is divided into two paths to be respectively communicated with a vacuum device and an empty valve. The synthesis device of the polyester polyol is characterized in that the intermediate tank filled with the water-absorbing substance is added between the reaction kettle and the reflux condenser. Compared with the traditional process device, the synthesis device has the advantages that the reaction speed is fast, the reaction time is short, the energy consumption is low, the equipment utilization rate is improved, the investment is saved, the wastewater treatment is simple and the treatment cost is low.

Description

technical field [0001] The invention belongs to the technical field of polyester polyol synthesis, in particular to a polyester polyol synthesis device. Background technique [0002] Polyester polyols are formed by polycondensation of small molecule polyols and dibasic acids. This is an equilibrium reversible reaction. During the reaction process, the small molecule water produced during the reaction must be continuously removed to disrupt the balance before the reaction can continue. To make the reaction proceed quickly, the reaction temperature must be increased and the water generated during the reaction must be removed in time. [0003] The dibasic acids used mainly include: [0004] (1) Saturated fatty acids: monooxalic acid, succinic acid, adipic acid, suberic acid, etc.; [0005] (2) Unsaturated fatty acids: maleic acid, fumaric acid, etc.; [0006] (3) Aromatic acids: terephthalic acid, isophthalic acid, phthalic acid or anhydrides. [0007] Polyols are: [0008...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/78
Inventor 陈海棠梅法洪
Owner 梅法洪
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