CN101279886B - Technological process for preparing durene with reformed C10 aromatic - Google Patents
Technological process for preparing durene with reformed C10 aromatic Download PDFInfo
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- CN101279886B CN101279886B CN2008100531861A CN200810053186A CN101279886B CN 101279886 B CN101279886 B CN 101279886B CN 2008100531861 A CN2008100531861 A CN 2008100531861A CN 200810053186 A CN200810053186 A CN 200810053186A CN 101279886 B CN101279886 B CN 101279886B
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- durol
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention relates to a technique for reforming a C10 arene to produce a durene, the reforming to the C10 arene undergoes steps of continuous rectification, freezing crystallization and separation by three rectification towers for separating out the durene front low-boiling fraction, rectifying out the durene liquid rich mother liquor and then extracting out the product before 205 DEG C by rectification; and the durene rich mother liquor is cooled to the temperature of between -5 and -10 DEG C through a refrigerating kettle, the durene in the rich liquid is saturated and separated out of a crystalline solid, and a solid durene product is obtained through fractional crystallization and pressure filtration. The product of the invention has the yield reaching 80 percent and the purity reaching 99 percent; and the technique is environment-friendly and energy-saving and will not produce smoke gas by applying the coal gas produced by itself. The technique has advantages of reducing the amount of freezing materials, increasing the freezing temperature and obviously saving the power, and has broad application prospect.
Description
Technical field
The present invention relates to extract in the aromatic hydrocarbons processing method of the method, particularly a kind of preparing durene with reformed C 10 aromatic of durol, specifically is the processing method that adopts three tower continuous rectifications, freezing and crystallizing and separation of produced durol.
Background technology
Durol (1) is a kind of important Organic Chemicals, and it produces pyromellitic acid anhydride (being called for short equal acid anhydride or PMDA) domestic main use, and PMDA is the important source material of synthesis of polyimides polymkeric substance.The production of China's durol also is in developmental stage, and major technique has: C
10The heavy aromatics perfectly crystallization process, unsym-trimethyl benzene methanol alkylation method, unsym-trimethyl benzene chloromethylation process, unsym-trimethyl benzene gas phase isomerization disproportionating method etc.Heavy aromatics perfectly crystallization process long flow path, production cost are higher; Unsym-trimethyl benzene chloromethylation process equipment corrosion is serious; Equal four technology are produced in the isomerization of unsym-trimethyl benzene disproportionation, and reaction conditions is had relatively high expectations, and need face the hydrogen pressurization and carry out, and this technology does not really realize suitability for industrialized production.
China CN 1048479A discloses a kind of reformation C+10 heavy aromatic hydrocarbon comprehensive utilization process and device, adopt efficient structured packing and condensing reflux to distribute the smart gold-plating that carries out program control intermittence or successive high-resolution degree of dissection in the efficient fractionate of control device, each gold-plating section fractional crystallization respectively then obtains products such as mixed methylnaphthalene and Rubber Softener and durol and refined naphthalene.
The enterprise of domestic production durol continues to use the old technology of the eighties exploitation always at present: the first, and need the refrigerated inventory big in the process of production durol, account for the 50-60% of total inventory greatly.The second, the freezing temp that requires in the process of production durol is low, for example will reach-35 ℃, and energy consumption is very high.The 3rd, the purity of product is low, generally at 93-94%, can not satisfy the demand of downstream unit.The 4th, the unstable product quality of old explained hereafter has caused detrimentally affect to the production of downstream producer.
Summary of the invention
The object of the present invention is to provide a kind of processing method of preparing durene with reformed C 10 aromatic, adopt the processing method of three tower continuous rectifications, freezing and crystallizing and separation of produced durol, can overcome the defective of prior art.Three tower continuous rectifications concentrate the durol pregnant solution, improve freezing temp, dwindle refrigerating apparatus and energy efficient, reduce production costs; Reduce the discharging of " three wastes ", improve production environment, have wide application prospect.
The processing method of a kind of preparing durene with reformed C 10 aromatic provided by the invention is the continuous rectification of reformed C 10 process, freezing and crystallizing, separating step:
1) reformed C 10 carries out continuous rectification through comprising rectifying tower T101, rectifying tower T201 and rectifying tower T301 at least, isolates the products before durol front low boiler cut, rectifying go out durol liquid enrichment mother liquor and rectifying proposes 205 ℃ again.
Said rectifying tower T101 master extracts the aromatic solvent before the durol, just S-100C.The T201 rectifying tower mainly is in order to extract the pregnant solution of durol, and main component is durol and isodurene.The content that can obtain durol is at 30%-45%.The T301 rectifying tower mainly is for the aromatic solvent before extracting 205 ℃, and improves the yield of aromatic solvent.
2) durol enrichment mother liquor cools to-5～-10 ℃ by freezing kettle, and preferred-7 ℃, xln is separated out in the satiety of the durol in the pregnant solution.
3) fractional crystallization in separating centrifuge.
4) through the pressure filter press filtration, obtain solid durol finished product.
The cat head working pressure of said rectifying tower T101 is 1～50kPa among the present invention, preferred 1～5kPa, 125～135 ℃ of cat head service temperatures, 150-170 ℃ of tower still service temperature.
The cat head working pressure of rectifying tower T201 is 1～50kPa, preferred 1～5kPa; 135～145 ℃ of cat head service temperatures, 180～190 ℃ of tower still service temperatures.
The cat head working pressure of T301 is 1～50kPa, preferred 1～5kPa.150-160 ℃ of cat head service temperature, 205-215 ℃ of tower still service temperature.
The present invention adopts the processing method of three tower continuous rectifications, freezing and crystallizing and separation of produced durol, can overcome the defective of prior art.Three tower continuous rectifications concentrate the durol pregnant solution, improve freezing temp, and dwindle refrigerating apparatus and reduced production cost, energy efficient, for example, the raw material per ton 35kw.h that can economize on electricity.20000 tons/year of annual processing, 700,000 kw.h that can economize on electricity save 420,000 yuan of the electricity charge.Reduce the discharging of " three wastes ", improve production environment.
Outstanding feature of the present invention is: (1) product yield height, and final product yield can reach 80%; And old technology has only 50%.(2) the purity height of product: adopt pre-separation, the purity of product is up to 99%; The purity of old Technology product is all below 95%.(3) environmental protection and energy saving: use the coal gas of oneself producing, can not produce flue dust.Reduce the refrigerated inventory and improved the refrigerated temperature, saved electric energy significantly; Old process technology equipment performance is bad, contaminate environment.The present invention has wide application prospect.
Description of drawings
Fig. 1 is heavy aromatics C10 three tower continuous rectification processing step device synoptic diagram of the present invention.
Fig. 2 is freezing, a centrifugal separation process step device synoptic diagram of the present invention.
Embodiment
Specific embodiments of the present invention is described in detail as follows with reference to accompanying drawing, but for illustrative purposes only rather than the restriction the present invention.
Fig. 1 is heavy aromatics C10 three tower continuous rectification processing step device synoptic diagram of the present invention.Fig. 2 is freezing, a centrifugal separation process step device synoptic diagram of the present invention.
As shown in the figure, T101 is a rectifying tower, and T201 is a rectifying tower, T301 is a rectifying tower, the 101st, and reformed C 10 raw material, the 102nd, durol front low boiler cut, the 103rd, the pregnant solution of the distillate durol of T201 rectifying tower, Room 104 are raffinates, 105 is the products before 205 ℃; The 10th, the pregnant solution 103,11st of the durol of desire refrigerated high density, cooling reactor, the 22nd, cooling reactor, the 33rd, cooling reactor, the 44th, separating centrifuge.
Refrigerating apparatus is the ice maker of selecting for use, and heat-transfer medium is the mixture of ethylene glycol and water.Centrifugation is that the centrifugal separator and the pressure filter series connection of selecting for use are used.
The raw material heavy aromatics obtains high equal four pregnant solutions of content by the three-tower rectification of Fig. 1.Said rectifying tower T101 mainly is to be aromatic solvent before the durol in order to extract durol front low boiler cut 102, just S-100C.Rectifying tower T201 mainly is in order to extract the pregnant solution of durol, and main component is durol and isodurene.The content of durol is at 30%-45%.Rectifying tower T301 mainly is in order to extract the products before 205 ℃, i.e. aromatic solvents before 205 ℃, and improve the yield of aromatic solvent.
The durol pregnant solution 103 of high density cools to-5～-10 ℃ by cooling reactor 11, freezing kettle 22, cooling 33 stills, and preferred-7 ℃, the supersaturation of the durol in the pregnant solution and separate out xln.The xln particle is bigger, and the centrifugation ratio is easier to.
By separating centrifuge 44 centrifugations, can obtain the solid durol of content 〉=85%.Then, 〉=85% solid durol enters pressure filter, carries out press filtration, obtains the solid durol finished product of content 〉=99%.
Application Example
Processing reformed C 10 (durol content 10% in the C10 aromatic hydrocarbons), enter 3000 kilograms/hour of the flow velocitys of rectifying tower T101 reformed C 10 raw material 101,600 kilograms/hour of the flow velocitys of durol front low boiler cut 102,600 kilograms/hour of the flow velocitys of the pregnant solution 103 of durol, 600 kilograms/hour of the flow velocitys of the product 105 before 205 ℃, 1200 kilograms/hour of the flow velocitys of the pregnant solution of the durol of high density (40-45%); 600 kilograms/hour of the flow velocitys of the pregnant solution 10 of the durol of desire refrigerated high density.
Operational condition (working pressure not specified otherwise all refers to absolute pressure):
Rectifying tower T101 cat head working pressure 2kPa, 132 ℃ of cat head service temperatures, 164 ℃ of tower still service temperatures.
Rectifying tower T201 cat head working pressure 2kPa, 141 ℃ of cat head service temperatures, 188 ℃ of tower still service temperatures.
Rectifying tower T301 cat head working pressure 2kPa, 155 ℃ of cat head service temperatures, 209 ℃ of tower still service temperatures.
Freezing kettle temperature-7 ℃.
Table 1 is that the present invention processes 1000 kilograms the reformed C 10 and the comparing result of old technology.
Table 1: the present invention processes 1000 kilograms the reformed C 10 and the comparing result of old technology.
| ? | Equal four pregnant solution output | Durol content | Freezing temp | Parting liquid durol content | Durol output | Energy expenditure |
| Old technology | 650kg | 15％ | -35℃ | 7％ | 52kg | 25350 kcal+97.5W phases |
| The present invention | 220kg | 43％ | -7℃ | 7％ | 79.2kg | 4884 kcal+94.6W phases |
The energy consumption of old technology: 650kgX0.6kcal/kgX (30 ℃-(35 ℃))+(650kgX15%XW phase)=25350kcal+97.5W phase.
Energy consumption of the present invention: 220kgX0.6kcal/kg X (30 ℃-(7 ℃))+(220kgX43%X W phase)=4884kcal+94.6W phase.
Old technology-the present invention=20466kcal+2.96W phase.
W phase: the heat of phase transformation of durol (liberated heat when durol changes from liquid into solid).
The raw material per ton 35kw.h that can economize on electricity, 20000 tons/year of the annual processing of this covering device.700,000 kw.h can economize on electricity.420,000 yuan of the annual saving electricity charge.
Claims (3)
1. the processing method of a preparing durene with reformed C 10 aromatic is passed through rectifying, freezing and crystallizing, separating step, it is characterized in that:
1) reformed C 10 is through comprising first rectifying tower (T101), second rectifying tower (T201) and the 3rd rectifying tower (T301) at least, carry out continuous rectification, isolate durol front low boiler cut, rectifying goes out durol liquid enrichment mother liquor, the product before rectifying proposes 205 ℃ again;
2) durol enrichment mother liquor cools to-7 ℃ by freezing kettle, and xln is separated out in the durol satiety in the pregnant solution;
3) fractional crystallization in separating centrifuge;
4) through the pressure filter press filtration, obtain solid durol finished product;
The cat head working pressure of said first rectifying tower (T101) is 1～50kPa, 125～135 ℃ of cat head service temperatures, 150-170 ℃ of tower still service temperature;
The cat head working pressure of said second rectifying tower (T201) is 1～50kPa, 135～145 ℃ of cat head service temperatures, 180～190 ℃ of tower still service temperatures;
The cat head working pressure of said the 3rd rectifying tower (T301) is 1～50kPa, 150-160 ℃ of cat head service temperature, 205-215 ℃ of tower still service temperature.
2. according to the said processing method of claim 1, it is characterized in that the content of durol of the overhead product of said second rectifying tower (T201) is 30-45%.
3. according to the said processing method of claim 1, it is characterized in that said separating centrifuge and pressure filter series connection use.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100531861A CN101279886B (en) | 2008-05-22 | 2008-05-22 | Technological process for preparing durene with reformed C10 aromatic |
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| CN2008100531861A CN101279886B (en) | 2008-05-22 | 2008-05-22 | Technological process for preparing durene with reformed C10 aromatic |
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| CN101279886A CN101279886A (en) | 2008-10-08 |
| CN101279886B true CN101279886B (en) | 2011-09-14 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103102239A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Method for continuous extraction of durene from C10 heavy aromatics |
| CN103351887B (en) * | 2013-07-08 | 2015-06-10 | 常熟市联邦化工有限公司 | Process for preparing high temperature heat transfer oil base oil by using C10 heavy aromatic residual oil |
| CN103524288B (en) * | 2013-09-30 | 2015-11-25 | 天津大学 | A kind of method of purification of durol |
| CN103864814B (en) * | 2014-02-24 | 2016-06-22 | 中国海洋石油总公司 | A kind of by the method preparing equal benzene tetramethyl acid anhydride in preparing gasoline by methanol artificial oil |
| CN105541543B (en) * | 2016-02-15 | 2018-03-13 | 天津市兴源化工有限公司 | The method of purification of durol |
| CN109970502A (en) * | 2017-12-28 | 2019-07-05 | 江苏正丹化学工业股份有限公司 | A kind of method of C10 aromartic isomerization production durol |
| CN109336728A (en) * | 2018-11-19 | 2019-02-15 | 鹏辰新材料科技股份有限公司 | A kind of process for effectively purifying of 1,2,4,5- durene |
| CN112876331B (en) * | 2021-02-05 | 2023-08-18 | 苏州久泰集团有限公司 | Method for producing durene |
| CN115417742B (en) * | 2022-09-05 | 2023-10-27 | 连云港鹏辰特种新材料有限公司 | Method for producing durene by fractional crystallization |
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2008
- 2008-05-22 CN CN2008100531861A patent/CN101279886B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| 赵银亮.碳十重芳烃综合利用工艺技术.《河南化工》.2003,(第8期),第24-25页，第26页2.2.3-2.2.5，图2. * |
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