CN107541345B - Recovery process of stearic acid hydrogenation catalyst - Google Patents
Recovery process of stearic acid hydrogenation catalyst Download PDFInfo
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- CN107541345B CN107541345B CN201711043062.0A CN201711043062A CN107541345B CN 107541345 B CN107541345 B CN 107541345B CN 201711043062 A CN201711043062 A CN 201711043062A CN 107541345 B CN107541345 B CN 107541345B
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Abstract
The invention relates to a recovery process of a stearic acid hydrogenation catalyst, which comprises the following steps: a. mixing and heating raw oil and a catalyst, and then feeding the mixture into a hydrogenation tower; b. pressurizing hydrogen to 2.0-2.3MPa, then entering a hydrogenation tower from the tower bottom, and carrying out hydrogenation reaction with the heated raw oil; c. the reaction product after hydrogenation reaction is led out from the top of the tower, cooled and then enters a thermal separation tank for gas-liquid separation, the liquid enters an intermediate tank, and the hydrogenated oil containing the catalyst in the intermediate tank is sent into a membrane concentration system through an oil transfer pump to concentrate the catalyst in the feed liquid. d. And conveying the catalyst concentrated solution to an air-cooled granulation tower of a granulation system, and granulating and recovering to obtain the catalyst embedded particles with the average particle size of 0.5-50 mm. The invention integrates the membrane technology, the granulation technology and the catalytic hydrogenation technology in the stearic acid production, realizes the recovery of the hydrogenation catalyst in an in-situ dispersion state by the integrated membrane technology adopted in the membrane concentration system, and has good economic and social benefits.
Description
Technical Field
The invention relates to the field, in particular to a recovery process of a stearic acid hydrogenation catalyst.
Background
Stearic acid (octadecanoic acid, C)18H36O2) Is important in modern industrial productionThe chemical raw materials are widely applied to synthesis and processing of plastics and rubber and production of stearate, and have important application in industrial fields such as daily chemistry, paint, oilfield chemistry and the like. As a high-grade saturated fatty acid, stearic acid is usually produced by taking oil as a raw material through links of catalytic hydrogenation, hydrolysis, distillation/rectification, hydrogenation and the like.
In the oil hydrogenation production process, a nickel catalyst is required to be added into the oil in proportion. After the hydrogenation is finished, the catalyst is separated from the hydrogenated oil and fat by a plate and frame filtration method. In the filtered catalyst filter cake, the catalyst can generate agglomeration, adhesion and other phenomena, and secondary pollution can also occur due to direct contact with air and other reasons in the processes of blanking collection, treatment and the like. In fact, the loss of catalytic activity of the catalyst includes two parts of adsorption poisoning and active site loss, and although the activity of the used catalyst is lost, the great activity is still remained, and the use value of the catalyst can be recovered by proper regeneration and activation treatment. The waste catalyst is a hazardous waste, seriously pollutes the environment, requires expensive disposal costs, and causes waste of resources.
One of the difficulties in recovering stearic acid hydrogenation catalyst is how to maintain its original dispersion state in the oil and fat, and avoid the adhesion and agglomeration caused by the compaction of the cake with piled particles. Therefore, the invention provides a scheme for recovering the in-situ dispersion state of the catalyst particles in the grease.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: in order to overcome the defects in the prior art, the invention provides a recovery process of a stearic acid hydrogenation catalyst, which aims to solve the problem of recovery of catalyst particles in oil in an in-situ dispersion state.
The technical scheme adopted by the invention for solving the technical problems is as follows: a recovery process of stearic acid hydrogenation catalyst comprises the following steps:
a. mixing the degassed raw oil with a catalyst, heating, and feeding into a hydrogenation tower;
b. pressurizing hydrogen to 2.0-2.3MPa by a compressor, then feeding the hydrogen into a hydrogenation tower from the tower bottom, and carrying out hydrogenation reaction on the hydrogen and the heated raw oil;
c. the reaction product after hydrogenation reaction is led out from the top of the tower, cooled and then enters a thermal separation tank for gas-liquid separation, the liquid and the liquid separated by the thermal separation tank are combined and enter a middle tank, and the hydrogenated oil containing the catalyst in the middle tank is sent into a membrane concentration system through an oil transfer pump to concentrate the catalyst in the feed liquid.
d. And conveying the catalyst concentrated solution to an air-cooled granulation tower of a granulation system, and granulating and recovering to obtain the catalyst embedded particles with the average particle size of 0.5-50 mm.
Preferably, in the step c, the membrane used in the membrane concentration system is an inorganic ceramic membrane or a metal membrane, and the average pore diameter of the membrane is 0.05-50 μm.
Further, in the step c, the driving force of the membrane separation process in the membrane concentration system comes from the pressure difference between the material from the hydrogenation tower and the membrane filtrate side, and the pressure difference range is 0.05-1 MPa.
Furthermore, in the step c, the membrane concentration system concentrates the catalyst in the feed liquid to the mass concentration of 1-50% under the conditions of the temperature range of 95-120 ℃ and the transmembrane pressure difference of 0.2-05 MPa.
The invention has the beneficial effects that: the invention integrates the membrane technology, the granulation technology and the catalytic hydrogenation technology in the stearic acid production, avoids the problem of waste catalyst generated by traditional plate-and-frame filtration by adopting the integrated membrane technology in the membrane concentration system, realizes the recovery of the hydrogenation catalyst in an in-situ dispersion state, and has good economic benefit and social benefit.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a block flow diagram of the recovery process of the present invention.
Detailed Description
The present invention will now be described in further detail with reference to the accompanying drawings. These drawings are simplified schematic views illustrating only the basic structure of the present invention in a schematic manner, and thus show only the constitution related to the present invention.
A recovery process of stearic acid hydrogenation catalyst comprises the following steps:
a. mixing the degassed raw oil with a catalyst, heating, and feeding into a hydrogenation tower;
b. pressurizing hydrogen to 2.0-2.3MPa by a compressor, then feeding the hydrogen into a hydrogenation tower from the tower bottom, and carrying out hydrogenation reaction on the hydrogen and the heated raw oil;
c. leading out a reactant after hydrogenation reaction from the top of the tower, cooling, then, introducing the reactant into a thermal separation tank for gas-liquid separation, combining the liquid with the liquid separated by the thermal separation tank, introducing the liquid and the liquid into an intermediate tank, and feeding the hydrogenated oil containing the catalyst in the intermediate tank into a membrane concentration system through an oil transfer pump to concentrate the catalyst in the feed liquid, wherein the membrane adopted in the membrane concentration system is an inorganic ceramic membrane or a metal membrane, and the average pore diameter of the membrane is 0.05-50 mu m; the driving force of the membrane separation process is derived from the pressure difference between the material from the hydrogenation tower and the membrane filtrate side, and the pressure difference range is 0.05-1 MPa; and finally, concentrating the catalyst in the feed liquid to a mass concentration of 1-50% in the temperature range of 95-120 ℃ and the transmembrane pressure difference condition of 0.2-05 MPa.
d. And conveying the catalyst concentrated solution to an air-cooled granulation tower of a granulation system, and granulating and recovering to obtain the catalyst embedded particles with the average particle size of 0.5-50 mm.
Example 1
Heating raw material palm oil from a raw material transfer tank through a pump and a feeding heat exchanger, then sending the raw material palm oil into a degassing tank, sending the degassed palm oil into a catalyst preparation tank, mixing the palm oil with a catalyst (5 mu m average particle size, framework nickel) (the weight ratio of the catalyst to grease is 1: 1000), heating to 200 ℃, and then sending the mixture into a hydrogenation tower. The hydrogen is pressurized to 2.0-2.3MPa by a compressor and then enters a hydrogenation tower together with the heated palm oil from the bottom of the tower for hydrogenation reaction, a reactant is led out from the top of the hydrogenation tower, is cooled by a finished product heat exchanger and a feed heat exchanger and then enters a thermal separation tank for gas-liquid separation, and liquid separated by the thermal separation tank enters an intermediate tank. And (3) feeding the hydrogenated oil containing the catalyst in the intermediate tank into a membrane concentration system through an oil transfer pump, wherein the membrane concentration system selects a ceramic membrane with the average pore diameter of 0.2 mu m, the catalyst in the feed liquid is concentrated to the mass concentration of 10% under the conditions of 120 ℃ and 0.2MPa transmembrane pressure difference, the concentrated solution of the catalyst is conveyed into an air-cooled granulation tower of a granulation system for granulation recovery, and the obtained catalyst embedded particles with the average particle size of 2mm are obtained.
Example 2
Heating raw material palm oil from a raw material transfer tank through a pump and a feeding heat exchanger, then sending the raw material palm oil into a degassing tank, sending the degassed palm oil into a catalyst preparation tank, mixing the palm oil with a catalyst (with the average particle size of 2 mu m and silicon dioxide loaded with nickel), heating to 200 ℃, and sending the mixture into a hydrogenation tower (the weight ratio of the catalyst to the grease is 1: 8000). Pressurizing hydrogen to 2.0-2.1MPa by a compressor, then feeding the hydrogen into a hydrogenation tower from the bottom of the tower for hydrogenation reaction, leading out reactants from the top of the tower, cooling, then carrying out gas-liquid separation, and feeding the liquid into an intermediate tank; and (3) feeding the hydrogenated oil containing the catalyst in the intermediate tank into a membrane concentration system through an oil transfer pump, wherein the membrane concentration system selects a stainless steel membrane with the average pore diameter of 0.1 mu m, the catalyst in the feed liquid is concentrated to the mass concentration of 20% under the conditions of 110 ℃ and 0.3MPa transmembrane pressure difference, and finally the catalyst concentrated solution is conveyed into an air-cooled granulation tower of a granulation system for granulation and recovery to obtain catalyst embedded particles with the average particle diameter of 5 mm.
Best mode for carrying out the invention
Heating raw oil, feeding into a degassing tank, mixing the degassed oil with a catalyst (10 μm average particle size, calcium-supported nickel) (catalyst: oil weight ratio 1: 8000), heating to 200 deg.C, and feeding into a hydrogenation tower; after the hydrogen is pressurized to 2.0-2.1MPa by a compressor, the hydrogen enters a hydrogenation tower from the bottom of the tower for hydrogenation reaction. Leading out a reactant from the top of the tower, cooling, then carrying out gas-liquid separation, and sending the hydrogenated oil containing the catalyst into a membrane concentration system by an oil transfer pump, wherein the membrane concentration system selects a porous titanium membrane with the average pore diameter of 1 mu m; concentrating the catalyst in the feed liquid to a mass concentration of 40% under the conditions of 95 ℃ and 0.5MPa transmembrane pressure difference; and conveying the concentrated catalyst solution to a water-cooling granulator of a granulating system for granulation and recovery to obtain catalyst embedded particles with the average particle size of 10 mm.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (4)
1. A recovery process of a stearic acid hydrogenation catalyst is characterized by comprising the following steps: comprises the following steps:
a. mixing the degassed raw oil with a catalyst, heating, and feeding into a hydrogenation tower;
b. pressurizing hydrogen to 2.0-2.3MPa by a compressor, then feeding the hydrogen into a hydrogenation tower from the tower bottom, and carrying out hydrogenation reaction on the hydrogen and the heated raw oil;
c. leading out the reactant after hydrogenation reaction from the top of the tower, cooling, then introducing the reactant into a thermal separation tank for gas-liquid separation, combining the liquid with the liquid separated by the thermal separation tank, introducing the liquid and the liquid into an intermediate tank, and feeding the hydrogenated oil containing the catalyst in the intermediate tank into a membrane concentration system through an oil transfer pump to concentrate the catalyst in the feed liquid;
d. and conveying the catalyst concentrated solution to an air-cooled granulation tower of a granulation system, and granulating and recovering to obtain the catalyst embedded particles with the average particle size of 0.5-50 mm.
2. The process for recovering a stearic acid hydrogenation catalyst according to claim 1, wherein: in the step c, the membrane adopted in the membrane concentration system is an inorganic ceramic membrane or a metal membrane, and the average pore diameter of the membrane is 0.05-50 mu m.
3. The process for recovering a stearic acid hydrogenation catalyst according to claim 2, wherein: in the step c, the driving force of the membrane separation process in the membrane concentration system comes from the pressure difference between the material from the hydrogenation tower and the membrane filtrate side, and the pressure difference range is 0.05-1 MPa.
4. A process for recovering a stearic acid hydrogenation catalyst according to claim 3, wherein: in the step c, the membrane concentration system concentrates the catalyst in the feed liquid to the mass concentration of 1-50% under the conditions of the temperature range of 95-120 ℃ and the transmembrane pressure difference of 0.2-05 MPa.
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| CN201711043062.0A CN107541345B (en) | 2017-10-31 | 2017-10-31 | Recovery process of stearic acid hydrogenation catalyst |
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| CN201711043062.0A CN107541345B (en) | 2017-10-31 | 2017-10-31 | Recovery process of stearic acid hydrogenation catalyst |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103113190A (en) * | 2013-02-05 | 2013-05-22 | 中国五环工程有限公司 | Butynediol low-pressure hydrogenation catalyst recycling process and system |
| CN103506165A (en) * | 2013-10-11 | 2014-01-15 | 中国海洋石油总公司 | Preparation method of large-aperture fat hydrogenation catalyst |
| CN103611581A (en) * | 2013-11-22 | 2014-03-05 | 中国天辰工程有限公司 | Method for recovering fine catalyst powder to repelletize |
| CN104368391A (en) * | 2014-11-10 | 2015-02-25 | 中国海洋石油总公司 | Hydrogenation catalyst with low trans-acid grease and preparation method thereof |
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- 2017-10-31 CN CN201711043062.0A patent/CN107541345B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103113190A (en) * | 2013-02-05 | 2013-05-22 | 中国五环工程有限公司 | Butynediol low-pressure hydrogenation catalyst recycling process and system |
| CN103506165A (en) * | 2013-10-11 | 2014-01-15 | 中国海洋石油总公司 | Preparation method of large-aperture fat hydrogenation catalyst |
| CN103611581A (en) * | 2013-11-22 | 2014-03-05 | 中国天辰工程有限公司 | Method for recovering fine catalyst powder to repelletize |
| CN104368391A (en) * | 2014-11-10 | 2015-02-25 | 中国海洋石油总公司 | Hydrogenation catalyst with low trans-acid grease and preparation method thereof |
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