CN204918420U - A device for preparing 1, 6 - hexanediol - Google Patents
A device for preparing 1, 6 - hexanediol Download PDFInfo
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- CN204918420U CN204918420U CN201520618722.3U CN201520618722U CN204918420U CN 204918420 U CN204918420 U CN 204918420U CN 201520618722 U CN201520618722 U CN 201520618722U CN 204918420 U CN204918420 U CN 204918420U
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Abstract
The utility model relates to a device for preparing 1, 6 - hexanediol belongs to the preparation technical field of 1, 6 - hexanediol. A device for preparing 1, 6 - hexanediol includes: esterification reaction device and hydrogenation device. Should be used for preparing the technology and the device of 1, 6 - hexanediol, and at first use 1, 6 - adipic acid and methyl alcohol to carry out esterification reaction as the raw materials in the esterification reaction device, obtain the dimethyl adipate, then dimethyl adipate and hydrogen carry out the electronation reaction in the hydrogenation device, finally obtain the 1, 6 - hexanediol, and the chromatogram content of 1, 6 - hexanediol is greater than 99.5%, have realized the industrial production of 1, 6 - hexanediol.
Description
Technical field
The utility model belongs to the preparing technical field of 1,6-hexylene glycol, is specifically related to a kind of device for the preparation of 1,6-hexylene glycol.
Background technology
Along with the develop rapidly of petrochemical complex, Fine Chemical and apparel industry, constantly expand by the range of application of 1,6-hexylene glycol synthesis product innovation, the demand of China to 1,6-hexylene glycol increases fast, and annual import volume increases with the ratio of more than 15%.
The hexylene glycol market in the current whole world is by BASF Aktiengesellschaft (BASF), Lanxess Corporation (former Beyer Co., Ltd) and Ube company monopolizing.The throughput that BASF Aktiengesellschaft has in Texas ,Usa free port and Ludwigshafen, Germany has reached 50,000 tons/year.There is 1,6-hexylene glycol product line device of ton in the Yu Bu company of Japan in Spain's construction, and Eastern Europe, South East Asia and China all never have the manufacturing enterprise forming mass-producing.China is 1, the production technology of 6-hexylene glycol is in open position always, and 1, the 6-hexylene glycol product that market needs all relies on from external import, based on brands such as Baeyer, German BASF (BASF) and Japanese space portions, annual import volume 3000-5000 ton.This will be that China faces important problem.
Utility model content
In order to solve the problems referred to above that prior art exists, the utility model provides a kind of device for the preparation of 1,6-hexylene glycol, to realize the suitability for industrialized production of 1,6-hexylene glycol.
The technical scheme that the utility model adopts is:
A kind of technique for the preparation of 1,6-hexylene glycol, it comprises: esterification device and hydrogenation reaction device;
Described esterification device comprise connect successively in order mixture tank, the first fresh feed pump, esterifier, in and pump, neutralization reactor, the first separating methanol pump, separating methanol distillation tower, dehydration pump, dehydration distillation tower, de-ester pump and de-ester distillation tower; The top of described separating methanol distillation tower is provided with the first condenser being connected with methyl alcohol holding tank, described dehydration distillation tower top is provided with the second condenser being connected with water collecting tank, and the top of described de-ester distillation tower is provided with the 3rd condenser being connected with ester holding tank;
Described hydrogenation reaction device comprise connect successively in order test tank, volume pump, hydrogen and material mixer, high pressure heat exchanger, hydrogenator, high-pressure separator, light pressure separator, the first water cooler, hold-up vessel, the second fresh feed pump, the first distillation tower, dealcoholysis pump and second column; Described test tank is connected with described ester holding tank;
Described hydrogenation reaction device also comprises make-up hydrogen compressor, circulating hydrogen compressor, methanol tank, dimethyl adipate storage tank and 1,6-hexylene glycol storage tank; Described separator is connected with described circulating hydrogen compressor, and described circulating hydrogen compressor is connected with described hydrogenation charging mixture tank; The top of described first distillation tower is provided with the second water cooler, described second water cooler is connected with described methanol tank and described dimethyl adipate storage tank respectively by sparger, the top of described second column is provided with the 3rd water cooler, described 3rd water cooler and described 1,6-hexylene glycol storage tank connect.
During use, by 1,6-hexanodioic acid and methyl alcohol are mixed with mixed solution by than row in mixture tank, then by the first fresh feed pump, the mixed solution prepared is made a gift to someone in esterifier, and esterification is there is under the effect of catalyst for esterification reaction and gac, obtain the reaction solution containing dimethyl adipate.Preferably, the consumption of gac accounts for 0.1% of raw material gross weight.
Reaction solution containing dimethyl adipate is pumped in neutralization reactor by neutralization, and in alkaline solution generation neutralization reaction, makes the basicity value that the reaction solution containing dimethyl adipate reaches suitable.The reaction solution containing dimethyl adipate regulating basicity value is pumped into separating methanol distillation tower by the first separating methanol, through the distillment of separating methanol distillation tower, is distilled away by methyl alcohol from tower top, and is collected in methyl alcohol holding tank through the effect of the first condenser.Bottom separating methanol distillation tower, remaining reaction solution is sent in dehydration distillation tower by dehydration pump, is distilled away at the top of water from dehydration distillation tower, and is collected in water collecting tank through the effect of the second condenser.Bottom dehydration distillation tower, remaining reaction solution is pumped in de-ester distillation tower by de-ester, dimethyl adipate becomes steam and steams from the top of de-ester distillation tower, then the effect through the 3rd condenser is collected in ester holding tank, thus obtains the higher dimethyl adipate of purity.
Passed in test tank by the dimethyl adipate prepared by esterification device, and prepare in proportion with methyl alcohol, be preferably, the weight ratio of dimethyl adipate and methyl alcohol is 1:1.
Mixed solution is by mixing with material mixer by hydrogen with the hydrogen after pressurization after volume pump boosting, then after high pressure heat exchanger heat temperature raising, hydrogenator is entered, issue raw reduction reaction in the effect of reducing catalyst, obtain the reaction solution containing 1,6-hexylene glycol.Hydrogen after pressurization, derives from through the new hydrogen of make-up hydrogen compressor pressurization and the recover hydrogen through circulating hydrogen compressor pressurization.
Containing 1, the reaction solution of 6-hexylene glycol makes residual hydrogen be separated with reaction solution through high-pressure separator and the effect of light pressure separator, to residual hydrogen recovery and by sending into the reaction continuing on for reduction dimethyl adipate in hydrogenation charging mixture tank after circulating hydrogen compressor pressurization.
Reaction solution after separation enters in hold-up vessel after the first water cooler cooling, then send in the first distillation tower by the second fresh feed pump, by the distillment of the first distillation tower, methyl alcohol and dimethyl adipate are steamed respectively from the top of the first distillation tower, and being collected in respectively in methanol tank and dimethyl adipate storage tank by sparger after cooling under the effect of the second water cooler, so that recycling.
Bottom first distillation tower, remaining reaction solution is pumped in second column by dealcoholysis, under the effect of second column, by 1,6-hexylene glycol distills from the tower top of second column, and be collected in 1,6-hexylene glycol storage tank after the 3rd water cooler cooling, obtain finished product.
Further, the agitator of described esterifier adopts grid agitator.
By grid agitator, 1,6-hexanodioic acid, methyl alcohol and 0.1% gac and catalyzer are fully stirred, thus be conducive to the carrying out of esterification.
Further, described methyl alcohol holding tank and described mixture tank, described methanol tank and described mixture tank, described dimethyl adipate storage tank is all connected by transferpump with between described test tank.
Recovery methyl alcohol in methyl alcohol holding tank is sent in mixture tank by transferpump, recovery methyl alcohol in methanol tank is sent in mixture tank by transferpump, recovery dimethyl adipate in dimethyl adipate storage tank is sent in test tank by transferpump, thus recovery methyl alcohol and dimethyl adipate are reused.
Further, the top of described de-ester distillation tower is provided with the first vacuum pump; The top of described second column is also provided with the second vacuum pump.
Reduce the pressure in de-ester vacuum column by the first vacuum pump, make the boiling point lowering of dimethyl adipate, thus be convenient to be distilled.Reduce the pressure in second column by the second vacuum pump, make the boiling point lowering of 1,6-hexylene glycol, thus be convenient to 1,6-hexylene glycol to distill.
The beneficial effects of the utility model are:
The device for the preparation of 1,6-hexylene glycol of the utility model by providing, is first that raw material carries out esterification in esterification device with 1,6-hexanodioic acid and methyl alcohol, obtains dimethyl adipate; Then dimethyl adipate and hydrogen carry out reduction reaction in hydrogenation reaction device, finally obtain 1,6-hexylene glycol, and the chromatographic content of 1,6-hexylene glycol is greater than 99.5%, achieve the suitability for industrialized production of 1,6-hexylene glycol.
Accompanying drawing explanation
Fig. 1 is the structural representation of the device for the preparation of 1,6-hexylene glycol described in embodiment.
Be labeled as in figure:
Mixture tank 101, first fresh feed pump 102, in and pump 103, neutralization reactor 104, first separating methanol pump 105, dehydration pump 106, de-ester pump 107, de-ester distillation tower 108, ester holding tank 109, first vacuum pump 110, 3rd condenser 111, water collecting tank 112, second condenser 113, dehydration distillation tower 114, methyl alcohol holding tank 115, first condenser 116, separating methanol distillation tower 117, esterifier 118, volume pump 119, hydrogen and material mixer 120, high pressure heat exchanger 121, first water cooler 122, hold-up vessel 123, second fresh feed pump 124, dealcoholysis pump 125, methanol tank 126, dimethyl adipate storage tank 127, second column 128, 1, 6-hexylene glycol storage tank 129, second vacuum pump 130, 3rd water cooler 131, sparger 132, second water cooler 133, first distillation tower 134, light pressure separator 135, high-pressure separator 136, hydrogenator 137, test tank 138, make-up hydrogen compressor 139, circulating hydrogen compressor 140.
Embodiment
Embodiment
As shown in Figure 1, provide a kind of device for the preparation of 1,6-hexylene glycol in the present embodiment, it comprises: esterification device and hydrogenation reaction device.
Esterification device comprise connect successively in order mixture tank 101, first fresh feed pump 102, esterifier 118, in and pump 103, neutralization reactor 104, first separating methanol pump 105, separating methanol distillation tower 117, dehydration pump 106, dehydration distillation tower 114, de-ester pump 107 and de-ester distillation tower 108; The top of separating methanol distillation tower 117 is provided with the first condenser 116 being connected with methyl alcohol holding tank 115, dehydration distillation tower 114 top is provided with the second condenser 113 being connected with water collecting tank 112, and the top of de-ester distillation tower 108 is provided with the 3rd condenser 111 being connected with ester holding tank 109; Esterifier 118 adopts grid agitator.
Hydrogenation reaction device comprise connect successively in order test tank 138, volume pump 119, hydrogen and material mixer 120, high pressure heat exchanger 121, hydrogenator 137, high-pressure separator 136, light pressure separator 135, first water cooler 122, hold-up vessel 123, second fresh feed pump 124, first distillation tower 134, dealcoholysis pump 125 and second column 128; Test tank 138 is connected with ester holding tank 109.
Hydrogenation reaction device also comprises make-up hydrogen compressor 139, circulating hydrogen compressor 140, methanol tank 126, dimethyl adipate storage tank 127 and 1,6-hexylene glycol storage tank 129; High-pressure separator 136 is all connected with circulating hydrogen compressor 140 with light pressure separator 135, and make-up hydrogen compressor 139 is all connected with material mixer 120 with hydrogen with circulating hydrogen compressor 140; The top of the first distillation tower 134 is provided with the second water cooler 133, second water cooler 133 is connected with methanol tank 126 and dimethyl adipate storage tank 127 respectively by sparger 132, the top of second column 128 is provided with the 3rd water cooler 131,3rd water cooler 131 and 1,6-hexylene glycol storage tank 129 connect.
For the ease of the recovery methyl alcohol in methyl alcohol holding tank 115 and methanol tank 126 is delivered in mixture tank 101, the dimethyl adipate in dimethyl adipate storage tank 127 is convenient to deliver in test tank 138, methyl alcohol holding tank 115 and mixture tank 101, methanol tank 126 and mixture tank 101, dimethyl adipate storage tank 127 is all connected by transferpump with test tank 138, therefore, directly transportation work is completed by transferpump.
As a kind of preferred version of the present embodiment, the top of de-ester distillation tower 108 is provided with the first vacuum pump 110; The top of second column 128 is also provided with the second vacuum pump 130.
Above-mentioned volume pump 119 is plunger type metering pump.
The utility model is not limited to above-mentioned preferred forms; anyone can draw other various forms of products under enlightenment of the present utility model; no matter but any change is done in its shape or structure; every have identical with the application or akin technical scheme, all drops within protection domain of the present utility model.
Claims (4)
1. one kind for the preparation of the device of 1,6-hexylene glycol, it is characterized in that, comprising: esterification device and hydrogenation reaction device;
Described esterification device comprise connect successively in order mixture tank, the first fresh feed pump, esterifier, in and pump, neutralization reactor, the first separating methanol pump, separating methanol distillation tower, dehydration pump, dehydration distillation tower, de-ester pump and de-ester distillation tower; The top of described separating methanol distillation tower is provided with the first condenser being connected with methyl alcohol holding tank, described dehydration distillation tower top is provided with the second condenser being connected with water collecting tank, and the top of described de-ester distillation tower is provided with the 3rd condenser being connected with ester holding tank;
Described hydrogenation reaction device comprise connect successively in order test tank, volume pump, hydrogen and material mixer, high pressure heat exchanger, hydrogenator, high-pressure separator, light pressure separator, the first water cooler, hold-up vessel, the second fresh feed pump, the first distillation tower, dealcoholysis pump and second column; Described test tank is connected with described ester holding tank;
Described hydrogenation reaction device also comprises make-up hydrogen compressor, circulating hydrogen compressor, methanol tank, dimethyl adipate storage tank and 1,6-hexylene glycol storage tank; Described high-pressure separator, described light pressure separator are all connected with described circulating hydrogen compressor, and described make-up hydrogen compressor, described circulating hydrogen compressor are all connected with material mixer with described hydrogen; The top of described first distillation tower is provided with the second water cooler, described second water cooler is connected with described methanol tank and described dimethyl adipate storage tank respectively by sparger, the top of described second column is provided with the 3rd water cooler, described 3rd water cooler and described 1,6-hexylene glycol storage tank connect.
2. the device for the preparation of 1,6-hexylene glycol according to claim 1, is characterized in that, the agitator of described esterifier adopts grid agitator.
3. according to claim 1 for the preparation of 1, the device of 6-hexylene glycol, is characterized in that, described methyl alcohol holding tank and described mixture tank, described methanol tank and described mixture tank, described dimethyl adipate storage tank is all connected by transferpump with between described test tank.
4. the device for the preparation of 1,6-hexylene glycol according to any one of claim 1-3, is characterized in that, the top of described de-ester distillation tower is provided with the first vacuum pump; The top of described second column is also provided with the second vacuum pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520618722.3U CN204918420U (en) | 2015-08-17 | 2015-08-17 | A device for preparing 1, 6 - hexanediol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520618722.3U CN204918420U (en) | 2015-08-17 | 2015-08-17 | A device for preparing 1, 6 - hexanediol |
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| Publication Number | Publication Date |
|---|---|
| CN204918420U true CN204918420U (en) | 2015-12-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201520618722.3U Expired - Fee Related CN204918420U (en) | 2015-08-17 | 2015-08-17 | A device for preparing 1, 6 - hexanediol |
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| Country | Link |
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| CN (1) | CN204918420U (en) |
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2015
- 2015-08-17 CN CN201520618722.3U patent/CN204918420U/en not_active Expired - Fee Related
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20151230 Termination date: 20180817 |
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| CF01 | Termination of patent right due to non-payment of annual fee |