CN101696168B - System and process for dehydrating and drying isooctyl nitrate crude product - Google Patents

System and process for dehydrating and drying isooctyl nitrate crude product Download PDF

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CN101696168B
CN101696168B CN200910218793.3A CN200910218793A CN101696168B CN 101696168 B CN101696168 B CN 101696168B CN 200910218793 A CN200910218793 A CN 200910218793A CN 101696168 B CN101696168 B CN 101696168B
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silica gel
slightly
crude product
essence
molecular sieve
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CN101696168A (en
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王育斌
曹彬
杨战厂
常兆军
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Xi'an Wonder Chemical Co Ltd
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Xi'an Wonder Chemical Co Ltd
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Abstract

The invention belongs to the technical field of producing petrochemicals such as nitrates, and specifically relates to a system and a process for dehydrating and drying an isooctyl nitrate crude product. The system and the process are to overcome the defect of low production efficiency in the prior art and adopt the following technical scheme: the system for drying the isooctyl nitrate crude product comprises a crude product tank, a rough-removing component, a fine-removing component and a product tank which are connected with a pump in turn, wherein the rough-removing component comprises two silica gel rough-removing devices connected in parallel, and the fine-removing component comprises one molecular sieve fine-removing device. The system and the process have the following advantages that: 1, the processing and the operation are simple and convenient; 2, the water content can be conveniently adjusted and controlled in real time as requested; 3, the used adsorbents are particles and have no problems of a sodium sulfate adsorbent which is easy to agglomerate after absorbing water and then increases the operational complexity; 4, the system and the process are stable and reliable; and 5, the production efficiency is greatly improved.

Description

A kind of dehydration drying system of isooctyl nitrate crude product and technique
Technical field
The invention belongs to the production technical field of petrochemicals nitric ether, be specifically related to a kind of dehydration drying system and technique of isooctyl nitrate crude product.
Background technology
Isooctyl ester nitrate is a kind of diesel cetane-number improver of excellent property.The nitrated method of industrial general employing isooctyl alcohol is produced.The method is taking the vitriol oil as catalyzer, by nitric acid and isooctyl alcohol after reactor is directly nitrated through separating, the operation such as alkali cleaning, washing and drying and dehydrating obtains product isooctyl ester nitrate.
The method of industrial main employing vacuum-drying at present and physical adsorption is dewatered.In CN1031525A, introduced a kind of synthesis technique, its drying and dehydrating workshop section mainly adopts vacuum drying method to dewater, and its weak point is to need special vaccum-pumping equipment, and investment and working cost are higher, are difficult to carry out.
CN1045773A discloses a kind of production technique and equipment, and this dewatering period process using oleophilic drainage material separation is dewatered, and its weak point is: the water separation capability of lipophilic material is poor, and the extremely low and quality product of production efficiency is more difficult reaches requirement.CN1903829A discloses a kind of dewatering process of isooctyl ester nitrate, its main points are to adopt settlement separate and anhydrous sodium sulphate physical adsorption to dewater, its weak point is: 1) adopt the method for slotting waddy to judge the degree of saturation of sorbent material, random large, be unfavorable for that industrial specification production and quality product control in real time.2) after anhydrous sodium sulphate water suction, very easily lump, hindered fluid flowing between sorbent material, reduced the service efficiency of sorbent material.3) inconvenience of the sodium sulfate after caking is dismantled, and has increased the trouble of step for regeneration.
Summary of the invention
The object of the invention is to propose a kind of dehumidification system and dewatering process of isooctyl nitrate crude product, the low problem of production efficiency existing to overcome prior art.
The problem existing for overcoming prior art, technical scheme provided by the present invention is: a kind of dehumidification system of isooctyl nitrate crude product, comprise thick products pot that pump connects successively, slightly de-assembly, the de-assembly of essence and products pot, described thick de-assembly comprises slightly de-device of two silica gel in parallel, and the de-assembly of described essence comprises a de-device of molecular sieve essence.
The built-in supporting framework of above-mentioned silica gel sparger, shell inner bottom part that slightly de-device and the de-device of molecular sieve essence arrange by columniform shell, shell internal upper part, the silk screen that the top of supporting framework arranges form, and silica gel is slightly placed particulate state discolour silica gel as dewatering agent on the silk screen of de-device; On the silk screen of the de-device of molecular sieve essence, place 5A sieve particle as dewatering agent.
Above-mentioned dewatering process is: the isooctyl nitrate crude product after washing slightly takes off the top of device through being pumped into silica gel from thick products pot, material after thick de-is slightly sent into the top of the de-device of molecular sieve essence in de-device bottom through pump from silica gel again, the finished product after dehydration from the bottom of the de-device of molecular sieve essence by being pumped in products pot.
Two above-mentioned silica gel slightly take off device simultaneously or independent use all can.
Above-mentioned material to be dried slightly sprays into through sparger at de-device top from silica gel, rely on gravity and system pressure to flow through adsorbent bed from top to bottom, material is sloughed in material to go out from thick de-device tower bottom flow after contained humidity by the physical adsorption of sorbent material, when silica gel slightly the silica gel of de-device bottom be changed to micro-when red by blueness, show that this slightly de-device internal adsorption agent has reached saturated, must take out and change, the silica gel after replacing can normal pressure or vacuum-drying reduction at 100~200 DEG C.
Material after above-mentioned thick taking off sprays into through sparger from the de-device of molecular sieve essence top, relies on gravity and system pressure to be flowed through from top to bottom adsorbent bed, and material is sloughed in material and entered products pot from smart de-device tower bottom flow after contained humidity by the physical adsorption of sorbent material; The moisture content of timing in testing product, to the sorbent material in the de-device of essence is changed and is regenerated, after replacing sorbent material can normal pressure or vacuum-drying reduction at 100~200 DEG C.
Key point of the present invention is to be divided into thick de-and Jing Tuoliangge workshop section by dehydrating operation, adopts jumbo discolour silica gel to slough most moisture in thick de-section, adopts the 5A molecular sieve of high adsorption capacity qualified to ensure product water content in the de-section of essence.The water-content that whole process system can regulate to control in product by material flow reaches specified requirement.
The invention has the advantages that:
1) required processing raw material and equipment with low cost, processing and simple to operation;
2) moisture content can facilitate the low real-time regulation and control that carries out as requested;
3) the sorbent used particle that is, without the problem that after sodium sulfate adsorbent water suction, easily caking causes Operating Complexity to increase;
4) when one of them silica gel is when slightly de-device internal adsorption agent must be changed regeneration, system feeding can be switched to another silica gel slightly de-device slightly take off, can effectively ensure that dehydration continous-stable carries out;
5) production efficiency significantly improves.
Brief description of the drawings:
Fig. 1 is the structural representation of system.
Reference numeral is as follows:
1-the first valve, 2-the second valve, 3-the 3rd valve, 4-the 4th valve, 5-the 5th valve, 6-the 6th valve, 7-the 7th valve, the thick products pot of 11-, 12-silica gel is de-device slightly, the de-device of 13-molecular sieve essence, 14-products pot
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in detail.
A dehumidification system for isooctyl nitrate crude product, comprises thick products pot 1 that pump connects successively, slightly de-assembly, the de-assembly of essence and products pot 4, and described thick de-assembly comprises slightly de-device 2 of two silica gel in parallel, and the de-assembly of described essence comprises a de-device 3 of molecular sieve essence.The built-in supporting framework of said silica gel sparger, shell inner bottom part that slightly de-device 2 and the de-device 3 of molecular sieve essence arrange by columniform shell, shell internal upper part, the silk screen that the top of supporting framework arranges form, and silica gel is slightly placed particulate state discolour silica gel as dewatering agent on the silk screen of de-device 2; On the silk screen of the de-device 3 of molecular sieve essence, place 5A sieve particle as dewatering agent.
Technique of the present invention is:
(1) isooctyl nitrate crude product after washing slightly takes off device 2 from thick products pot 1 through being pumped into silica gel, material to be dried slightly sprays into through sparger at de-device 2 tops from silica gel, rely on gravity and system pressure to be flowed through from top to bottom adsorbent bed, material is sloughed in material to go out from thick de-device tower bottom flow after contained humidity by the physical adsorption of sorbent material.
When silica gel slightly the silica gel of de-device 2 bottoms be changed to micro-ly when red by blueness, show that this slightly de-device internal adsorption agent has reached saturated, must take out and change, the silica gel after replacing can normal pressure or vacuum-drying reduction at 100~200 DEG C.Said two silica gel slightly de-device 2 one-piece constructions can to adopt synthetic glass be that material processes, simultaneously or separately use all can.
(2) material after thick taking off is slightly sent into the smart top that takes off device 3 of molecular sieve in de-device 2 bottoms through pump from silica gel again, spray into through sparger, rely on gravity and system pressure to be flowed through from top to bottom adsorbent bed, material is sloughed in material and is entered products pot 4 from the de-device tower bottom flow of essence after contained humidity by the physical adsorption of sorbent material.Moisture content in timing testing product, to change and regenerate the sorbent material in the de-device of essence.After replacing sorbent material can be at 100~200 DEG C normal pressure or vacuum-drying reduction.
Referring to Fig. 1, further illustrate as follows:
1, open the first valve 1, the 3rd valve 3, close the second valve 2, the 4th valve 4, the 5th valve 5, the 6th valve 6, the 7th valve 7.Open pump, material after dehydration is sent into the slightly de-device 12 of silica gel that installs in advance discolour silica gel from the first valve 1, silica gel slightly the material of de-device 12 from the 3rd valve 3 through being pumped into the de-device 13 of molecular sieve essence that installs in advance 5A molecular sieve, dry after finished product from the de-device 13 of molecular sieve essence from the 7th valve 7 through being pumped into finished pot 14.
2, when silica gel slightly in de-device 12 80% sorbent material color be changed to when pale red by indigo plant, open the second valve 2, the 4th valve 4, close the first valve 1, the 3rd valve 3, charging is switched to another silica gel and slightly takes off device 12.Open the 5th valve 5, emit the slightly de-interior remaining liq of device 12 of silica gel, after liquid is emitted completely; Open slightly de-device 12 spigot discharges of silica gel, emit saturated adsorbers, and add fresh dried agent.The dry regeneration of RS Regenerator Section is delivered in the saturated adsorption agent drawing off.
3, timing detects water-content in the rear one-tenth of dehydration, and corresponding adjustment liquid phase flow or sorbent material, makes product water content meet up-to-standard requirement.

Claims (4)

1. the dewatering process of the dehumidification system of an isooctyl nitrate crude product, described dehumidification system comprises thick products pot (11) that pump connects successively, slightly de-assembly, the de-assembly of essence and products pot (14), described thick de-assembly comprises slightly de-device (12) of two silica gel in parallel, and the de-assembly of described essence comprises a de-device (13) of molecular sieve essence; The built-in supporting framework of described silica gel sparger, shell inner bottom part that slightly de-device (12) and the de-device (13) of molecular sieve essence arrange by columniform shell, shell internal upper part, the silk screen that the top of supporting framework arranges form, and silica gel slightly takes off on the silk screen of device (12) places particulate state discolour silica gel as dewatering agent; On the silk screen of the de-device (13) of molecular sieve essence, place 5A sieve particle as dewatering agent, the dewatering process of the dehumidification system of described isooctyl nitrate crude product, it is characterized in that: the isooctyl nitrate crude product after washing slightly takes off the top of device (12) through being pumped into silica gel from thick products pot (11), material after thick de-is slightly sent into the top of the de-device (13) of molecular sieve essence in de-device (12) bottom through pump from silica gel again, the finished product after dehydration from the bottom of the de-device (13) of molecular sieve essence by being pumped in products pot (14).
2. the dewatering process of the dehumidification system of a kind of isooctyl nitrate crude product as claimed in claim 1, is characterized in that: two described silica gel slightly take off device (12) simultaneously or independent use all can.
3. the dewatering process of the dehumidification system of a kind of isooctyl nitrate crude product as claimed in claim 2, it is characterized in that: described material to be dried slightly sprays into through sparger at de-device (12) top from silica gel, rely on gravity and system pressure to flow through adsorbent bed from top to bottom, material is sloughed in material to go out from thick de-device tower bottom flow after contained humidity by the physical adsorption of sorbent material, when silica gel slightly the silica gel of de-device (12) bottom be changed to micro-when red by blueness, show that this slightly de-device internal adsorption agent has reached saturated, must take out and change, silica gel after replacing can normal pressure or vacuum-drying reduction at 100 ~ 200 DEG C.
4. the dewatering process of the dehumidification system of a kind of isooctyl nitrate crude product as claimed in claim 3, it is characterized in that: the material after described thick taking off sprays into through sparger from the de-device (13) of molecular sieve essence top, rely on gravity and system pressure to be flowed through from top to bottom adsorbent bed, material is sloughed in material and is entered products pot from the de-device tower bottom flow of essence after contained humidity by the physical adsorption of sorbent material; The moisture content of timing in testing product, to the sorbent material in the de-device of essence is changed and is regenerated, after replacing sorbent material can normal pressure or vacuum-drying reduction at 100 ~ 200 DEG C.
CN200910218793.3A 2009-11-04 2009-11-04 System and process for dehydrating and drying isooctyl nitrate crude product Active CN101696168B (en)

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CN107011247B (en) * 2017-05-05 2019-12-06 利安隆凯亚(河北)新材料有限公司 Process for removing water and salt in triacetonamine synthetic liquid by using adsorbent
CN112441879B (en) * 2020-12-10 2022-07-22 山东泰和水处理科技股份有限公司 Method for synthesizing dichloropropanol
CN115014050A (en) * 2021-03-03 2022-09-06 上海交通大学 Agricultural product low-temperature adsorption drying and heat pump desorption coupling system and method for using same

Citations (5)

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Publication number Priority date Publication date Assignee Title
US4448587A (en) * 1983-03-28 1984-05-15 Ethyl Corporation Synergistic cetane improver
EP0129995A2 (en) * 1983-06-24 1985-01-02 Aeci Limited A process for the manufacture of nitric acid esters
CN1869000A (en) * 2006-06-27 2006-11-29 山东联合化工股份有限公司 Cleaning technology of iso-octly nitrate crude product
CN1903829A (en) * 2006-06-27 2007-01-31 山东联合化工股份有限公司 Dewater technology of isooctyl nitrate
CN101462962A (en) * 2007-12-19 2009-06-24 中国科学院大连化学物理研究所 Method for synthesizing isooctyl nitrate and microchannel reactor

Patent Citations (5)

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Publication number Priority date Publication date Assignee Title
US4448587A (en) * 1983-03-28 1984-05-15 Ethyl Corporation Synergistic cetane improver
EP0129995A2 (en) * 1983-06-24 1985-01-02 Aeci Limited A process for the manufacture of nitric acid esters
CN1869000A (en) * 2006-06-27 2006-11-29 山东联合化工股份有限公司 Cleaning technology of iso-octly nitrate crude product
CN1903829A (en) * 2006-06-27 2007-01-31 山东联合化工股份有限公司 Dewater technology of isooctyl nitrate
CN101462962A (en) * 2007-12-19 2009-06-24 中国科学院大连化学物理研究所 Method for synthesizing isooctyl nitrate and microchannel reactor

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Title
Hashimoto, Koutarou等.The study on cetane number improvement of diesel fuel.《Nippon Enerugi Gakkaishi》.1995,第74卷(第4期),第200-4页.
HZSM-5催化剂上硝酸酯对烷基苯的选择性硝化;彭新华等;《南京理工大学学报》;19991231;第23卷(第6期);第504-505页 *
The study on cetane number improvement of diesel fuel;Hashimoto, Koutarou等;《Nippon Enerugi Gakkaishi》;19951231;第74卷(第4期);第200-4页 *
彭新华等.HZSM-5催化剂上硝酸酯对烷基苯的选择性硝化.《南京理工大学学报》.1999,第23卷(第6期),第504-505页.

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