Method for preparing polyester thermosol

A polyester hot-melt adhesive and prepolymer technology, applied in adhesives, etc., can solve problems such as low recycling value, environmental pollution, and increased product costs, and achieve the effects of reducing waste water discharge, reducing costs, and ensuring stability

Active Publication Date: 2008-02-20
南通天洋光伏材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] When dimethyl terephthalate and glycol are transesterified, methanol will be produced as a by-product, and methanol has a low boiling point and is volatile and causes environmental

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0028] Example 1

[0029] Terephthalic acid (199.2g) and 1,4-butanediol (140.4g) were added into a 1.0L beating kettle, and after stirring and beating, nitrogen was continuously pressed into the 1.0L esterification kettle (3g / min). The kettle is equipped with a stirring and temperature measuring system, a rectification column and a reflux condenser, and ethylene terephthalate prepolymer (40g, molecular weight 500-600) and titanium / tin composite catalyst are pre-filled in the kettle [C 4 H 9 OSnOOH / Ti(OOC 4 H 9 ) 4 =1] (0.36g), the temperature in the control still under normal pressure is 195 DEG C to carry out an esterification, the generated water is recovered through the rectification system, the rectification reflux ratio is 3.5, and the column top vapor temperature is 100 DEG C, After the slurry is added, the reaction is continued until the vapor phase temperature at the top of the column drops significantly, and the primary esterification reaction ends.

[0030] Afte...

Example Embodiment

[0032] Example 2

[0033] Put terephthalic acid (199.2g), 1,4-butanediol (135g) and ethylene glycol (12.4g) into a 1.0L beating kettle. After stirring and beating, continuously press in with nitrogen (3g / min) In the 1.0L esterification kettle, ethylene terephthalate prepolymer (MW500) (45g) and titanium / tin composite catalyst [C 4 H 9 OSnOOH / Ti(OOC 3 H 7 ) 4 =1] (0.28g), the temperature in the esterification kettle is controlled to be 175°C under normal pressure, the reflux ratio of the rectification system is about 3.5, the vapor phase temperature at the column top is 100°C, and the slurry is added and the reaction is continued until the top of the column. When the vapor phase temperature drops significantly, the first esterification reaction ends.

[0034] After adding isophthalic acid (179.2g), azelaic acid (18.8g), 1,4-butanediol (90g) and 1,4-cyclohexanedimethanol (30g) to the beating kettle, stirring and beating, nitrogen It was continuously pressed into the above-...

Example

[0036] Examples 3 to 8

[0037] According to the same steps and conditions of Example 1, the difference is that the ratio of the raw materials used is shown in Table 1, and the characteristic parameters of the obtained product are also listed in Table 1.

[0038] Table 1 Material ratio and product performance of Examples 3-8 (in Table 1, the material ratio is in mole percent)

[0039] Example number

[0040] Zinc acetate

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PUM

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Abstract

The invention discloses a preparation method of polyester hot melt adhesive, comprising the steps that: (1) A phthalic acid and a dihydric alcohol are mixed and beaten; next an esterification reactor is put into the beaten mixture continuously; a prepolymer of phthalic acid and a dihydric alcohol as well as titanium KEYI tin are added in the esterification reactor in advance; the reaction temperature is between 160 DEG C and 205 DEG C; at the same time, the water generated from the reaction process is discharged, then an esterification process is carried out for the first time; (2) An isophthalic acid, an aliphatic dicarboxylic acid and a diol are mixed and beaten again, next, the beaten mixture is put into an esterification reactor continuously, the reaction temperature is between 185 DEG C and 225 DEG C, then, the esterification process is carried out for the second time, meanwhile, the water generated from reaction process is discharged; after that, a polycondensation catalyst and other auxiliary are added in the esterification reactor for decompression and polycondensation at the temperature between 220 DEG C and 250 DEG C for 0.5 to 1.5 hours ,thereby the thepolyester hot melt adhesive product is obtained. The producing of by-product methanol is avoided and the cost of production is lowered by using the method. By adopting the continuous feeding method of sterification, the stability products are ensured and the discharging of waste water is decreased.

Description

technical field [0001] The invention relates to a preparation method of polyester hot melt adhesive. Background technique [0002] Polyester hot-melt adhesive has the characteristics of good melting fluidity, fast curing speed, high bond strength, impact resistance, and bending resistance. It is one of the hot-melt adhesive varieties with the best heat resistance. It is suitable for metals, ceramics, glass, Cement, wood, and plastics have relatively satisfactory adhesion, and are especially suitable for industries such as fiber, clothing, electrical appliances, and shoemaking. [0003] At present, polyester hot-melt adhesives are mostly obtained by polycondensation of diol esters of terephthalic acid, diol esters of isophthalic acid, and diol esters of long-chain aliphatic dibasic acids. The glycol ester of dicarboxylic acid is then obtained by transesterification of dimethyl terephthalate and corresponding glycol, as USP 6,255,443 proposes to synthesize a kind of low-melti...

Claims

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Application Information

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IPC IPC(8): C09J167/03C08G63/181C08G63/85
Inventor 曾作祥黄海南李哲龙朱万育陶思玉马志艳
Owner 南通天洋光伏材料科技有限公司
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