CN101040674A - Method for producing food level liquid carbon dioxide product - Google Patents
Method for producing food level liquid carbon dioxide product Download PDFInfo
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- CN101040674A CN101040674A CNA200710200557XA CN200710200557A CN101040674A CN 101040674 A CN101040674 A CN 101040674A CN A200710200557X A CNA200710200557X A CN A200710200557XA CN 200710200557 A CN200710200557 A CN 200710200557A CN 101040674 A CN101040674 A CN 101040674A
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Abstract
The invention relates to a method for producing edible liquid carbon dioxide product, characterized in that in compression step, the distribution of the third-stage outlet gas of compressor is adjusted by an adjusting valve, to supply needed thermal source to distillation via the compressed gas transmitted to a purifying tower, in the purifying step, some carbon dioxide gas and foul gas of purifying tower are discharge from tower top as splash steam to be throttled, expanded and reduced temperature via an adjusting valve A, to be feedback to a heat exchanger at the upper part of the purifying tower, to exchange heat with ascending splash steam in tube, and reduce pressure to 0.05MPa via an adjusting valve B, to be feed into purifying process to exchange heat with material gas to recycle cold as the regenerated gas of purifying or drying process. The invention uses adjusting valves A, B to control pressure discharge of purifying tower, to assure the stable pressure of purifying tower. The recycle rate of carbon dioxide of invention is at least improved 3%, while the consumption is at least reduced 5% and the carbon dioxide can reach the standard of edible carbon dioxide.
Description
Technical field
The present invention relates to is a kind of production method of food level liquid carbon dioxide product.
Background technology
Carbon dioxide is important industrial production raw material, be widely used in fields such as metallurgy, iron and steel, oil, chemical industry, electronics, food, medical treatment, has purposes widely at aspects such as food industry applications especially, the controlled atmosphere of food, the application of beverage industry, food refrigerated and freezing application, supercritical extract etc.Can two big classes be arranged for the carbon dioxide enriched source of the gas that industry is reclaimed, be Natural carbon dioxide gas source and industrial by-product source of the gas carbon dioxide, Natural carbon dioxide gas originates in some gas field, in the alive boundary stone oil and gas recovery process, find many carbon dioxide or carbon dioxide enriched gas field, its carbon dioxide content is 15 ~ 99%.On Chinese Guangdong, Shandong and Jiangsu and other places, there is high concentration carbon dioxide gas field with value of exploiting and utilizing.The own purity height of some Natural carbon dioxide gas body (carbonated is about 99%), utilize well head pressure through the dedusting drying, but remove just packing commercial Application behind heavy hydrocarbon and the sulfide, but generally only limit to commercial Application, as produce food-grade carbon-dioxide, then need further refining.Also recyclable carbon dioxide both can reach the comprehensive utilization carbon resource from the byproduct source of the gas of various industrial process, can administer the environmental pollution that brings because of industrial gas emission again.The by-product source of the gas is mainly from following industrial processes, such as the fermentation waste gas of the decarbonization gas of synthesis ammonia plant, Alcohol Plant, blast furnace gas, lime-kiln gas, flue gas etc.At present, people more and more recognize excessive carbon dioxide are put in the atmosphere in vain, have both wasted resource, cause environmental pollution again, and be made into food-grade carbon-dioxide, not only can increase benefit, also help enterprise and adjust the product mix, promote that enterprise develops to product diversification.China is that world's carbon dioxide mainly discharges one of state.Therefore, do the comprehensive utilization of carbon dioxide well,, transform mode of economic growth, build resource-conserving and environment amity society, alleviate shortage of resources contradiction and environmental pressure, promote that the harmony between man and nature development is significant developing a circular economy.Past is restricted by technology of preparing and market, and China's food-grade carbon-dioxide evaluation and exploration technology is also relatively backward.Simultaneously, China's food-grade carbon-dioxide product standard is not in line with international standards fully, only requires the content of carbon dioxide, and is not tight to the content requirement of trace impurity wherein, differs greatly with international standard.It is very strict that the food-grade carbon-dioxide international standard requires, and it is 20 multinomial, wherein very high to the purity requirement of carbon dioxide that index has, and a lot of impurity contents all require to be lower than ppm or ppb level.Therefore, the preparation food-grade carbon-dioxide difficulty that can meet international standards is very big.
The method of carbon dioxide recovery mainly contains solvent-recovery process, cryogenic rectification method, absorption method, membrane separation process and compression condensation method etc., but all adopts the compression condensation method usually.The compression condensation method is that carbon dioxide is compressed to 2MPa-8MPa, is divided into high-pressure process and middle-pressure process by its pressure again, and high-pressure process pressure is had relatively high expectations, and uses water cooling after the compression at normal temperatures, makes co 2 liquefaction, perhaps directly irritates to steel cylinder with gas form.This method requires compressor pressure than higher, it is more to consume energy, simultaneously because the system pressure height, require also high to whole pipe and container, investment and operating cost increase, and the purifying carbon dioxide difficulty is strengthened, and carbon dioxide purity is not high, be difficult to satisfy the demand of market, transport and store cumbersome in addition high-pureness carbon dioxide.Another is a middle-pressure process, replaces water-cooled to come liquefied carbon dioxide with artificial cooling, can solve the deficiency that said method exists, and only carbon dioxide need be compressed to more than the 2.2MPa, with refrigeration machine carbon dioxide is cooled to-15 ℃ of pacts then and makes it liquefaction.Refrigeration unit that though whole system is many like this, system pressure reduces greatly, and compressor unit's wasted work is descended, and the requirement of withstand voltage of equipment, pipeline is low, purifies easily, and the carbon dioxide quality improves, and transportation is stored convenient, has better superiority.The patent No. 00116187.3 has been introduced a kind of production method of food-class liquid CO 2, production technology is technologies such as purification process, drying, liquefaction such as unstripped gas compression, desulfurization, carbon dioxide after the liquefaction has directly entered the product storage tank, can obtain the liquid CO 2 of certain purity by this method, but may have N owing to not removing fully effectively in the unstripped gas
2, H
2, CH
4Deng component, these components belong to light component, be not easy liquefaction, can be dissolved in the liquid CO 2 a certain amount ofly, make the quality of product carbon dioxide be affected, this invention does not simultaneously have the cold in the abundant removal process, causes energy consumption bigger, does not meet the thinking of development of present energy-saving and cost-reducing, recycling economy; Application number 200610092071.4 has been introduced a kind of with potash complex liquid absorbing carbon dioxide, and the method for carbon dioxide is produced in desorb from absorption liquid then, and the rate of recovery of this method is not high, has the easy loss of absorption liquid, secondary pollution, the more high shortcoming of energy consumption simultaneously.
Summary of the invention
The objective of the invention is to be improved, innovate at shortcoming that exists in the background technology and problem, provide a kind of processing technology routine advanced person, reliable, product quality is easy to control, production efficiency high and have the production method of energy-saving and cost-reducing a kind of food-class liquid CO 2.
Technical solution of the present invention is: it comprises following production stage:
(1) it will enter feed gas compressor from the CO 2 raw material gas of battery limit (BL) after wash and precooling, the process separator is removed mechanical water, be pressurized to 2.0-3.0MPa through three grades of compressions, and the gas that comes out cools off through cooler;
(2) cooled unstripped gas enters clarifier, by being filled with aluminium oxide, or active carbon, or silica gel, or the adsorbent of molecular sieve adsorbs;
(3) unstripped gas that comes from cleaning procedure enters drier, removes moisture content;
(4) flashed vapour that comes out of dried gas and purifying column top is after the heat exchanger heat exchange, and cooled gas enters evaporative condenser and liquefies;
(5) carbon dioxide after the liquefaction enters purifying column and distills purification, obtains liquid CO 2 in tower still bottom;
(6) enter the storage of liquid CO 2 basin at last.
The further technical solution of the present invention is: it comprises following production stage:
(1) it will be from the CO 2 raw material gas of battery limit (BL) through washing and precooling, entering feed gas compressor after removing mechanical water through separator, is pressurized to 2.0-3.0MP through three grades of compressions, the gas that comes out through cooler carry out cold promptly;
(2) cooled unstripped gas enters clarifier, by being filled with aluminium oxide, or active carbon, or silica gel, or the adsorbent of molecular sieve adsorbs;
(3) unstripped gas that comes from cleaning procedure enters drier, removes moisture content;
(4) flashed vapour that comes out of dried gas and purifying column top is after the heat exchanger heat exchange, and cooled gas enters evaporative condenser and liquefies;
(5) carbon dioxide after the liquefaction enters purifying column and distills purification, obtains liquid CO 2 in tower still bottom;
(6) enter the storage of liquid CO 2 basin at last;
Be characterized in: in compression step, the distribution of three grades of exit gas of compressor is regulated by control valve, makes to be delivered to the purifying column Compressed Gas fractionation required thermal source of purifying fully is provided; In purification step, a part of carbon dioxide and incoagulable gas in the purifying column are discharged by cat head, be called flash steam, this flashed vapour temperature after control valve A throttling expansion reduces, return the heat exchanger shell pass on purifying column top, with the flashed vapour heat exchange that tube side rises, after control valve B is depressurized to about 0.05MPa once more, delivers to cleaning procedure and unstripped gas heat exchange and reclaim the regeneration gas that cold is used as purification or drying process then.Divide the pressure releasing of two sections control purifying columns by control valve A, B, guarantee the stable of purifying column operating pressure.
The present invention has following advantage and effect:
The one, utilize the thermal source of a part of unstripped gas of three grades of outlets of compressor as the purifying column reboiler, the carbon dioxide and the impurity of not liquefaction and the trace impurity that is dissolved in the liquid CO 2 are discharged from the purifying column top after suitably adding thermal distillation, can reduce the extraneous thermal source of reboiler, help improving the quality of carbon dioxide simultaneously.The 2nd, make full use of expand the carbon dioxide degree of depth cooling that the cold that produces goes out to flash distillation and make it to liquefy again of purifying column top second throttle, reduce the consumption of energy liquefied ammonia, reach the rate of recovery that improves carbon dioxide and the purpose of energy savings.After adopting the present invention, the rate of recovery of carbon dioxide in the identical unstripped gas is improved more than 3% at least, energy consumption simultaneously reduces at least 5%, load the fully standard of food-grade carbon-dioxide of resulting carbon dioxide.
Description of drawings
Accompanying drawing is a process flow diagram of the present invention
The specific embodiment
1, unstripped gas compression
According to the unstripped gas of outside the battery limit (BL), sending here that is rich in carbon dioxide of unstripped gas through washing and precooling, after removing mechanical water, the process separator enters feed gas compressor, be pressurized to 2.0-3.0MPa through three grades of compressions, from three grades of unstripped gas that come out of compressor, sub-fraction is delivered to the thermal source of the purifying column of condensation purification process as reboiler, most of gas cools off through three grades of outlet aftercoolers of compressor, delivers to the oil removing cleaning procedure then.
The distribution of three grades of exit gas of compressor is regulated by control valve, makes to be delivered to the purifying column Compressed Gas fractionation required thermal source of purifying fully is provided.This is one of characteristics of the present invention.Can certainly adopt other source of the gas to replace this Compressed Gas, but from aspect such as energy-saving and cost-reducing certainly not as the present invention.
2, cleaning procedure
The gas that three grades of aftercoolers of compressed machine come out is introduced into the water cooler cooling, enters cleaning procedure then with after another strand unstripped gas that returns after the purifying column heat exchange mixes.
Cleaning procedure is made up of 2-6 platform clarifier, this operation is mainly removed in the unstripped gas may contain the impurity that heavy hydrocarbon, alcohols, sulfide etc. influence the carbon dioxide quality, according to factors such as the size of raw gas flow, content, this operation can be by 2-6 platform clarifier, simultaneously according to the difference of unstripped gas impurities kind, can distinguish in the clarifier or load a kind of or several adsorbents in aluminium oxide, active carbon, silica gel, the molecular sieve simultaneously.
This operation adopts temperature swing adsorption process, its principle be utilize the selective absorption of ABSORBENTS ABSORPTION hydrocarbon, alcohols, sulfide etc. and adsorbent to the adsorption capacity of gas with various along with the difference of temperature has characteristic than big-difference, normal temperature adsorbs impurity, high temperature desorption impurity, reaches the purpose of gas purification.Many clarifier switch operatings, when a certain or several clarifiers were in adsorbed state, remaining clarifier then was in regeneration step.Heating and the regeneration gas of using during cold blowing are mainly come the flashed vapour of autocondensation purification process, the flashed vapour that comes from the condensation purification process earlier with the heat exchange of dried raw material gas reclaim be with cold after, as the regeneration gas of clarifier adsorbent is regenerated.Absorption and recovery time are generally 4-48 hour, the setting of time is mainly according to factors such as the size of unstripped gas actual flow, impurity contents, because there is the ability of relatively-stationary processing impurity in adsorbent, if traffic load is big and impurity content when big, then adsorption time is answered corresponding shortening, the then corresponding corresponding shortening of recovery time meeting; If traffic load is little and impurity content hour, then adsorption time should corresponding prolongation, and the then corresponding recovery time can corresponding prolongation.
The absorption of adsorbent, following five steps of the main process of regeneration:
(1) absorption (A)
Unstripped gas enters adsorption tower from the bottom or the top of adsorption tower, discharge from the other end of adsorption tower, in adsorption tower, ABSORBENTS ABSORPTION hydrocarbon, alcohols, sulfide etc. effectively adsorb, make indexs such as heavy hydrocarbon in the gas of the port of export, alcohols, sulfide reach respective design index or required standard, after being adsorbed to certain hour, estimate that adsorbent stops absorption when saturated.
(2) the reverse pressure (D) of putting
After adsorption step finishes, adsorption tower inner high voltage gas is discharged outside the clarifier against the release of absorption direction current limliting, the pressure that finishes the back adsorption tower is near normal pressure.
(3) add thermal desorption impurity (H)
Being used to can be as the gas of regeneration gas from the flashed vapour at the purifying column top of rectification and purification operation or other, after the heat exchanger heat exchange, enter electric heater then to be heated to～160 ℃ enter the absorber that is in the thermal regeneration step, direction flushing adsorbent against absorption, make the impurity of its absorption be heated desorb, adsorbent is fully regenerated, then as toxic emission.
(4) cooling adsorbent (C)
After thermal regeneration finished, the impurity in the clarifier almost obtained complete desorb, can utilize this moment without heating from the flashed vapour at the purifying column top of rectification and purification operation will or other can clarifier be cooled to≤40 ℃ as the gas of regeneration gas.
(5) clarifier pressurising (R)
Utilize the part of all the other clarifiers that are in adsorbed state this clarifier to be pressurized to adsorptive pressure, prepare to enter absorption next time through the gas after the purified treatment.
In this operation, as because of less flashed vapour quantity not sufficients that causes from the rectification and purification operation of hydrogen component content such as the nitrogen in the unstripped gas, hydrogen, methane, can't be in setting-up time with the clarifier heating or be cooled to require temperature, thereby when needing to increase regeneration tolerance, can select the regeneration gas as a supplement of dropping a hint of carbon dioxide storage tank for use, if tolerance is still not enough, then can replenish little air or other gas as regeneration gas.
With two clarifier (A
#, B
#) technology experience absorption (A), step-down (D) successively, heating (H), cold blowing (C) in circulation once, boost (R) totally five steps be example time-scale is as follows:
Alternating temperature absorption time-scale
| 1 | 2 | |||||||
| A # | A | D | H | C | R | |||
| B # | D | H | C | R | A | |||
3, drying process
The unstripped gas that comes from cleaning procedure enters drier, removes institute's water content, delivers to the heat exchanger of cleaning procedure and carries out heat exchange to reduce temperature with flashed vapour from rectification and purification operation purifying column, delivers to the condensation operation then.The design of drier or operation quantity can be 2-6 platform absorber according to the traffic load size and the water content of unstripped gas, are filled with adsorbents such as silica gel, molecular sieve in every drier.This operation still adopts the technology of alternating temperature absorption, and the regeneration gas that heating or cold blowing are used is air or other suitable source of the gas.
4, liquefaction operation
The flashed vapour that comes out from the gas and the purifying column top of drying process is after the heat exchanger heat exchange, the evaporative condenser that cooled gas enters this operation liquefies, the low-temperature receiver of this operation is from the liquefied ammonia freezing process, in evaporative condenser, carbon dioxide fully and liquefied ammonia carry out exchange heat, liquefied ammonia liquid level in the evaporative condenser is accurately controlled by control valve, and most carbon dioxide is fully liquefied, and sends into purification process then.
5, purification process
Liquid CO 2 from the liquefaction operation enters purifying column and distills purification, obtain the product liquid carbon dioxide in tower still bottom, liquid CO 2 is delivered to subcooler after control valve 1 control step-down, in subcooler, the product carbon dioxide that part gasifies because of step-down is liquefied again to improve recovery rate of CO 2, fluid temperature also further reduces, and the product carbon dioxide is delivered to the product storage tank that product is stored operation through sequencing valve.
A part of carbon dioxide and incoagulable gas in the purifying column are discharged by cat head, be called flash steam, this flashed vapour temperature after control valve A throttling expansion reduces, return the heat exchanger shell pass on purifying column top, flashed vapour heat exchange with the tube side rising, after control valve B is depressurized to about 0.05MPa once more, delivers to cleaning procedure and unstripped gas heat exchange and reclaim the regeneration gas that cold is used as the dealcoholysis operation then.Divide the pressure releasing of two sections control purifying columns by control valve A, B, guarantee the stable of purifying column operating pressure.This technology is one of characteristics of the present invention, its objective is to reach the rate of recovery that improves carbon dioxide, reduce cold consumption, fully guarantee the quality of liquid CO 2.
The rectifying principle is adopted in the design of purifying column, adopts the coil pipe heat exchange structure at the bottom of the tower, with a part of unstripped gas carbon dioxide liquid in tower chassis pipe heating tower, reaches the effect that improves purifying column tower bottoms body carbon dioxide purity.Cat head is the tubular heat exchanger structure, and the top flashed vapour is cooled to-40 ℃ approximately through throttling, with the mixed gas converting heat that contains part gas phase carbon dioxide and incoagulable gas of pact-10～-15 of rising ℃, to reclaim carbon dioxide wherein.As flashed vapour cold deficiency, be to improve the rate of recovery, the condensation of liquefying of available a small amount of liquefied ammonia.
Product purity is by regulating the control of flash distillation tolerance, CH in product
4, N
2, when CO etc. exceeds standard, need to increase flash distillation tolerance, advance purifying column bottom heating tolerance and can increase flash distillation tolerance by increasing.The heating tolerance of reboiler is regulated by the control valve of compression section.
6, storage procedure
From the product carbon dioxide liquid of rectification and purification operation, deliver to the storage of liquid CO 2 basin.
Embodiment of the present invention only is the description that preferred implementation of the present invention is carried out; be not that design of the present invention and scope are limited; do not breaking away under the preceding topic of design philosophy of the present invention; engineers and technicians make technical scheme of the present invention in this area various modification and improvement; all should fall into protection scope of the present invention; the technology contents that the present invention asks for protection all is documented in claims.
Claims (2)
1. the production method of a food level liquid carbon dioxide product is characterized in that it comprises following production stage:
(1) will be from the CO 2 raw material gas outside the battery limit (BL) through washing and precooling, after removing mechanical water, the process separator enters feed gas compressor, be pressurized to 2.0-3.0MPa through three grades of compressions, the gas that comes out cools off through cooler;
(2) cooled unstripped gas enters clarifier, by being filled with aluminium oxide, or active carbon, or silica gel, or the adsorbent of molecular sieve adsorbs;
(3) unstripped gas that comes from cleaning procedure enters drier, removes moisture content;
(4) flashed vapour that comes out of dried gas and purifying column top is after the heat exchanger heat exchange, and cooled gas enters evaporative condenser and liquefies;
(5) carbon dioxide after the liquefaction enters purifying column and distills purification, obtains liquid CO 2 in tower still bottom;
(6) enter the storage of liquid CO 2 basin at last.
2. the production method of a food level liquid carbon dioxide product, it comprises following production stage:
(1) will be from the CO 2 raw material gas outside the battery limit (BL) through washing and precooling, after removing mechanical water, the process separator enters feed gas compressor, be pressurized to 2.0-3.0MPa through three grades of compressions, the gas that comes out cools off through cooler;
(2) cooled unstripped gas enters clarifier, by being filled with aluminium oxide, or active carbon, or silica gel, or the adsorbent of molecular sieve adsorbs;
(3) unstripped gas that comes from cleaning procedure enters drier, removes moisture content;
(4) flashed vapour that comes out of dried gas and purifying column top is after the heat exchanger heat exchange, and cooled gas enters evaporative condenser and liquefies;
(5) carbon dioxide after the liquefaction enters purifying column and distills purification, obtains liquid CO 2 in tower still bottom;
(6) enter the storage of liquid CO 2 basin at last;
It is characterized in that: in compression step, the distribution of three grades of exit gas of compressor is regulated by control valve, makes to be delivered to the purifying column Compressed Gas distillation required thermal source of purifying fully is provided; In purification step, a part of carbon dioxide and incoagulable gas in the purifying column are discharged by cat head, be called flash steam, this flashed vapour temperature after control valve A throttling expansion reduces, return the heat exchanger shell pass on purifying column top, with the flashed vapour heat exchange that tube side rises, after control valve B is depressurized to about 0.05MPa once more, delivers to cleaning procedure and unstripped gas heat exchange and reclaim the regeneration gas that cold is used as purification or drying process then.Divide the pressure releasing of two sections control purifying columns by control valve A, B, guarantee the stable of purifying column operating pressure.
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Assignee: Anqing KMT Gas Co., Ltd. Assignor: Hunan kaimeite gas Limited by Share Ltd|Sichuan Kaiyuan Technology Co., Ltd. Contract record no.: 2011340000107 Denomination of invention: Method for producing food level liquid carbon dioxide product Granted publication date: 20101201 License type: Exclusive License Open date: 20070926 Record date: 20110708 |