CN103288579A - Liquid benzene low-temperature purification method - Google Patents
Liquid benzene low-temperature purification method Download PDFInfo
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- CN103288579A CN103288579A CN2012100518064A CN201210051806A CN103288579A CN 103288579 A CN103288579 A CN 103288579A CN 2012100518064 A CN2012100518064 A CN 2012100518064A CN 201210051806 A CN201210051806 A CN 201210051806A CN 103288579 A CN103288579 A CN 103288579A
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Abstract
The invention relates to a liquid benzene low-temperature purification method. A raw material benzene is added into a reactor containing a purification agent so as to remove the race amounts of sulphur, arsenic, basic nitrogen, aromatic hydrocarbons with the carbon atom number of more than 9 and tar in the raw material benzene; the raw material benzene comprises the following components: 3-15mg/kg of the sulphur, 1-10mg/kg of the basic nitrogen, 0.1-1.5mg/kg of the arsine, 20-100mg/kg of diisopropylbenzene, 20-100mg/kg of triisopropyl benzene and 10-50mg/kg of the tar; and the operation temperature is 15-40 DEG C, and the liquid space velocity is 0.7-2.0/h. The method has low purification operation temperature, a good effect and multiple functions, is used for purifying the raw material benzene for cumene production, can also be used for regenerating hot benzene washing liquid for cumene production and recycles the benzene in the hot benzene washing liquid, and the removal rates of the trace mounts of the sulphur, the arsenic, the basic nitrogen, the aromatic hydrocarbons with the carbon atom number of more than 9 and the tar in the benzene reach 99.8%.
Description
Technical field:
The present invention relates to a kind of method of liquid benzene low temperature purification, exactly relate to take off Determination of Trace Sulfur in a kind of liquid benzene, take off micro amount of arsenic, take off micro-basic nitrogen, the method for the low temperature purification of the above aromatic hydrocarbons of C9 and tar etc.
Background technology
In the phenol production process, mostly be to adopt the alkylation reaction of benzene and propylene and diisopropylbenzene(DIPB) or/and the dealkylation reaction of tri-isopropyl benzene, produce isopropyl benzene, adopt acid β or MCM-22 molecular sieve as the catalyzer of synthesizing iso-propylbenzene at the alkylation reaction of benzene and propylene, in order to guarantee catalyzer long period, steady running, the Determination of Trace Sulfur in benzene feedstock, benzene alkene and the systemic circulation benzene, micro amount of arsenic, micro-basic nitrogen, the above aromatic hydrocarbons of micro-C9 and micro-tar are purified.Processing requirement C
8+ aromatic content≤20mg/kg, basic nitrogen≤1mg/kg sulphur≤3mg/kg, hydrogen arsenide+hydrogen sulfide≤100 μ g/kg, though single desulfurizing agent, single smart dearsenic agent, the single scavenging agent developmental level of taking off basic nitrogen agent and the above aromatic hydrocarbons of the single C9 of taking off and tar are higher, to these several a kind of scavenging agents that all work of above processing requirement do not appear in the newspapers so far to.Hydrocarbonylation catalyzer in the isopropyl benzene production process is regenerated after 2-3 time, and catalyzer just becomes waste residue to be handled.When using β type or modification beta molecular sieve as the hydrocarbonylation catalyzer, wash regeneration every carrying out hot benzene the 3-4 month, each hot benzene is washed the benzene that all must consume the 100-120 ton, and the benzene of its small part carries out rectifying through the recycle benzene tower and reclaims, recycling, most of as low-quality benzene take-away.Benzene major impurity after hot benzene is washed is the arsenic 1mg/kg of the micro-above aromatic hydrocarbons 0.5% of C9, tar 0.001%, little sulphur content 5mg/kg, trace, these impurity make the hydrocarbonylation catalyst deactivation, these impurity are deviate from, and the benzene after hot benzene is washed carries out alkylation reaction as raw material again.Reduce the production cost of isopropyl benzene.Adopt single scavenging agent to connect, need four kinds of single scavenging agents, complex process, equipment are many, and troublesome poeration is economical unreasonable.At present, existing micro-sweetening agent, micro-dearsenic agent, trace take off the basic nitrogen agent, all need be 100-120 ℃ of operation.In explained hereafter, need a kind of scavenging agent that Determination of Trace Sulfur in the benzene, micro amount of arsenic, micro-basic nitrogen, the above aromatic hydrocarbons of micro-C9 and micro-tar are purified.
Summary of the invention
The object of the invention is to provide a kind of method of liquid benzene low temperature purification, deviates from Determination of Trace Sulfur, micro amount of arsenic, micro-basic nitrogen, the above aromatic hydrocarbons of micro-C9 and micro-tar in the liquid benzene.
The technical solution used in the present invention is as follows:
Feed benzene feedstock in the reactor that scavenging agent is housed and remove Determination of Trace Sulfur, micro amount of arsenic, micro-basic nitrogen, the above aromatic hydrocarbons of micro-C9 and micro-tar in the benzene feedstock; Sulphur content 3～15mg/kg in the benzene feedstock, basic n content 1～10mg/kg, hydrogen arsenide content 0.1～1.5mg/kg, diisopropylbenzene(DIPB) content 20～100mg/kg, tri-isopropyl benzene content 20～100mg/kg, tar content 10～50mg/kg;
Service temperature is 15-40 ℃, liquid air speed 0.7～2.0h
-1
Scavenging agent is:
In HMCM-49, HMCM-22, the H beta-molecular sieve one or both or three kinds of adding sesbania powder mix with mass content 5-10% aqueous nitric acid, through rolling, granulation, extruded moulding is at 100-120 ℃ of dry 12-24h, at 500-560 ℃ of roasting 8-15h, make.
The sesbania powder that adds 1-5kg in every 100kg molecular sieve.
Add 110-130kg mass content 5-10% aqueous nitric acid in every 100kg molecular sieve.
Molecular sieve is any two kinds in HMCM-49, HMCM-22, the H beta-molecular sieve, and any molecular sieve quality accounts for the 0.3-0.75 of total mass.
Molecular sieve is three kinds in HMCM-49, HMCM-22, the H beta-molecular sieve, and these three kinds of molecular sieve mass ratioes are HMCM-49: HMCM-22: H β=2-4: 2-4: 6-2.
The present invention is used for the purification of benzene, has multiple functions such as the Determination of Trace Sulfur of deviating from, micro amount of arsenic, micro-basic nitrogen, the above aromatic hydrocarbons of micro-C9 and micro-tar.Scavenging agent specific surface area provided by the invention is greater than 400m
2g
-1, pore volume (0.58cm
3.g
-1), total acid content 0.38mmol/g because scavenging agent provided by the invention belongs to molecular sieve, has big surface-area, also has the electric charge of height concentration of local simultaneously, and the electric charge of these concentration of local makes molecular sieve polarity or polarizable compound such as H be arranged strong adsorption
2S and arsenic etc. and then play the effect of micro-desulfurization and dearsenification.Scavenging agent provided by the invention has surface acidity, and micro-basic nitrogen is had neutralizing effect, can be used for taking off basic nitrogen; The MCM that has or beta-molecular sieve structure have adsorption to the above aromatic hydrocarbons of micro-C9 and micro-tar in the benzene.
The present invention can be applicable to the purification of the benzene feedstock that isopropyl benzene produces, and also can be used for the regeneration that hot benzene is washed in the isopropyl benzene production, reclaims the benzene of hot benzene in washing, and reduces and produces the isopropyl benzene cost.
The service temperature of liquid benzene low temperature purification provided by the invention agent is 15-40 ℃, is almost room temperature.Service temperature is low to be the characteristics of maximum of the present invention.
Embodiment
[embodiment 1]
With the HMCM-49 molecular sieve that research institute of oily Jilin Petrochemical company among the 100kg produces, add 2kg sesbania powder, add the aqueous nitric acid of 130kg mass content 8%, roll evenly extrusion, 100 ℃ of dry 16h, 540 ℃ of roasting 12h at rolling machine.Make full-service fluid benzene scavenging agent.
Get Jilin Petrochemical company dye processing plant benzene feedstock, the content 99.8% of benzene, C
8+ aromatic content≤20mg/kg, sulphur≤3mg/kg, basic nitrogen≤1mg/kg, hydrogen arsenide+hydrogen sulfide≤0.1mg/kg, feed hydrogen arsenide, hydrogen sulfide and ammonia to benzene successively, make the sulphur content in the benzene feedstock be transferred to 15mg/kg, basic n content is transferred to 10mg/kg, hydrogen arsenide content is transferred to 1.5mg/kg, adds diisopropylbenzene(DIPB), tri-isopropyl benzene and tar in benzene feedstock, with diisopropylbenzene(DIPB) content 100mg/kg, tri-isopropyl benzene content 100mg/kg, tar content 50mg/kg.
Get dried present embodiment low temperature purification agent 100g, pack into
In the reactor, at 22 ℃, liquid air speed 2.0h
-1Following benzene from volume pump to reactor that squeeze into allotment with, take a sample at the reactor middle outlet, use the graphite furnace atomic absorption spectrometry micro amount of arsenic, with potentiometric determination trace basic nitrogen, use ultraviolet fluorescence method, measure Determination of Trace Sulfur, kapillary look-matter coupling analytical procedure is adopted in the analysis of diisopropylbenzene(DIPB), tri-isopropyl benzene and tar
Its detected result such as following table one.
The evaluation result of table one 1# low temperature purification agent
[embodiment 2]
With the H beta-molecular sieve that oily Jilin Petrochemical research institute of company and Dalian University of Science ﹠ Engineering among the 100kg are produced, add 5kg sesbania powder, add the aqueous nitric acid of 120kg mass content 5%, roll evenly extrusion, 120 ℃ of dry 18h, 530 ℃ of roasting 15h at rolling machine.Make the agent of full-service fluid benzene low temperature purification.
Adopt raw material and the method for [embodiment 1], with the low temperature purification agent of [embodiment 2], at 25 ℃, liquid air speed 1.0h
-1, its detected result sees Table two.
The evaluation result of table two 2# low temperature purification agent
[embodiment 3]
With the HMCM-22 molecular sieve that research institute of oily Jilin Petrochemical company among the 100kg produces, add 1kg sesbania powder, add the aqueous nitric acid of 120kg mass content 5%, roll evenly extrusion, 110 ℃ of dry 12h, 560 ℃ of roasting 8h at rolling machine.Make the agent of full-service fluid benzene low temperature purification.
Adopt raw material and the method for [embodiment 1], with the low temperature purification agent of [embodiment 3], at 25 ℃, liquid air speed 1.5h
-1, its detected result sees Table three.
The evaluation result of table three 3# low temperature purification agent
[embodiment 4]
The H beta-molecular sieve that oily Jilin Petrochemical research institute of company and Dalian University of Science ﹠ Engineering are produced among the HMCM-49 molecular sieve that research institute of oily Jilin Petrochemical company among the 30kg is produced, the HMCM-22 molecular sieve that 30kg Jilin University produces and the 40kg mixes, add 2kg sesbania powder, the aqueous nitric acid that adds 130kg mass content 8%, roll evenly at rolling machine, extrusion, dry 16h under 100 ℃, 540 ℃ of roasting 12h.Make the agent of full-service fluid benzene low temperature purification.
Adopt raw material and the method for [embodiment 1], with the low temperature purification agent of [embodiment 4], at 30 ℃, liquid air speed 1.1h
-1, its detected result sees Table four.
The evaluation result of table four 4# low temperature purification agent
[embodiment 5]
The HMCM-49 molecular sieve that research institute of oily Jilin Petrochemical company among the 60kg is produced, the HMCM-22 molecular sieve that 40kg Jilin University produces mix, add 2kg sesbania powder, the aqueous nitric acid that adds 130kg mass content 8%, roll evenly at rolling machine, extrusion, 100 ℃ of dry 16h, 540 ℃ of roasting 12h.Make the agent of full-service fluid benzene low temperature purification.
Adopt raw material and the method for [embodiment 1], with the low temperature purification agent of [embodiment 5], at 30 ℃, liquid air speed 0.9h
-1, its detected result sees Table five.
The evaluation result of table five 5# low temperature purification agent
[embodiment 6]
H beta-molecular sieve and 60kgHMCM-22 molecular sieve that oily Jilin Petrochemical research institute of company and Dalian University of Science ﹠ Engineering among the 40kg are produced mix, and add 5kg sesbania powder, add the aqueous nitric acid of 120kg mass content 5%, roll evenly at rolling machine, extrusion, 120 ℃ of dry 18h, 530 ℃ of roasting 15h.Make the agent of full-service fluid benzene low temperature purification.
Adopt raw material and the method for [embodiment 1], with the low temperature purification agent of [embodiment 6], at 30 ℃, liquid air speed 0.9h
-1, its detected result sees Table six.
The evaluation result of table six 6# low temperature purification agent
[embodiment 7]
Benzene when getting the Jilin Petrochemical company hot benzene in dye processing plant and washing, the content 99.5% of benzene, the content 0.15% of isopropyl benzene, diisopropylbenzene(DIPB) 0.12%, tar content 0.009%, sulphur content 11mg/kg, basic n content 3mg/kg, hydrogen arsenide content 0.9mg/kg, low temperature purification agent with [embodiment 1], at 23 ℃, liquid air speed 1.3h
-1, its detected result sees Table seven.
The evaluation result of the benzene low temperature purification agent when table seven is washed with hot benzene
Claims (5)
1. the method for a liquid benzene low temperature purification is characterized in that:
Feed benzene feedstock in the reactor that scavenging agent is housed and remove Determination of Trace Sulfur, micro amount of arsenic, micro-basic nitrogen, the above aromatic hydrocarbons of micro-C9 and micro-tar in the benzene feedstock; Sulphur content 3～15mg/kg in the benzene feedstock, basic n content 1～10mg/kg, hydrogen arsenide content 0.1～1.5mg/kg, diisopropylbenzene(DIPB) content 20～100mg/kg, tri-isopropyl benzene content 20～100mg/kg, tar content 10～50mg/kg; Service temperature is 15-40 ℃, liquid air speed 0.7～2.0h
-1
Scavenging agent is:
In HMCM-49, HMCM-22, the H beta-molecular sieve one or both or three kinds of adding sesbania powder mix with mass content 5-10% aqueous nitric acid, through rolling, granulation, extruded moulding is at 100-120 ℃ of dry 12-24h, at 500-560 ℃ of roasting 8-15h, make.
2. method according to claim 1 is characterized in that: the sesbania powder that adds 1-5kg in every 100kg molecular sieve.
3. method according to claim 1 is characterized in that: add 110-130kg mass content 5-10% aqueous nitric acid in every 100kg molecular sieve.
4. method according to claim 1, it is characterized in that: molecular sieve is any two kinds in HMCM-49, HMCM-22, the H beta-molecular sieve, and any molecular sieve quality accounts for the 0.3-0.75 of total mass.
5. method according to claim 1, it is characterized in that: molecular sieve is three kinds in HMCM-49, HMCM-22, the H beta-molecular sieve, these three kinds of molecular sieve mass ratioes are HMCM-49: HMCM-22: H β=2-4: 2-4: 6-2.
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|---|---|---|---|
| CN2012100518064A CN103288579A (en) | 2012-03-01 | 2012-03-01 | Liquid benzene low-temperature purification method |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08325176A (en) * | 1995-05-31 | 1996-12-10 | Sumitomo Chem Co Ltd | Purification of meta-diisopropylbenzene |
| CN1228073A (en) * | 1996-08-20 | 1999-09-08 | 陶氏化学公司 | Process for production of alkylated benzenes |
| CN1344703A (en) * | 2001-09-28 | 2002-04-17 | 北京石油化工学院 | Prepn of sulfurless benzene with pyrolytic light benzol |
| CN1461290A (en) * | 2000-08-16 | 2003-12-10 | 埃克森美孚化学专利公司 | Method for removal of polar contaminants from aromatic feedstocks |
| CN1918092A (en) * | 2003-12-19 | 2007-02-21 | 环球油品有限责任公司 | Process and apparatus for the removal of nitrogen compounds from a fluid stream |
-
2012
- 2012-03-01 CN CN2012100518064A patent/CN103288579A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08325176A (en) * | 1995-05-31 | 1996-12-10 | Sumitomo Chem Co Ltd | Purification of meta-diisopropylbenzene |
| CN1228073A (en) * | 1996-08-20 | 1999-09-08 | 陶氏化学公司 | Process for production of alkylated benzenes |
| CN1461290A (en) * | 2000-08-16 | 2003-12-10 | 埃克森美孚化学专利公司 | Method for removal of polar contaminants from aromatic feedstocks |
| CN1344703A (en) * | 2001-09-28 | 2002-04-17 | 北京石油化工学院 | Prepn of sulfurless benzene with pyrolytic light benzol |
| CN1918092A (en) * | 2003-12-19 | 2007-02-21 | 环球油品有限责任公司 | Process and apparatus for the removal of nitrogen compounds from a fluid stream |
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Application publication date: 20130911 |