CN114349629B - A system and process for recovering sodium acetate from oil by-products - Google Patents
A system and process for recovering sodium acetate from oil by-products Download PDFInfo
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- 235000017281 sodium acetate Nutrition 0.000 title claims abstract description 167
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 title claims abstract description 165
- 239000001632 sodium acetate Substances 0.000 title claims abstract description 165
- 238000000034 method Methods 0.000 title claims abstract description 90
- 230000008569 process Effects 0.000 title claims abstract description 89
- 239000006227 byproduct Substances 0.000 title claims abstract description 18
- 239000007864 aqueous solution Substances 0.000 claims abstract description 116
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 70
- 238000001704 evaporation Methods 0.000 claims abstract description 46
- 230000008020 evaporation Effects 0.000 claims abstract description 46
- 238000004042 decolorization Methods 0.000 claims abstract description 45
- 238000001914 filtration Methods 0.000 claims abstract description 29
- 238000010979 pH adjustment Methods 0.000 claims abstract description 25
- 230000002378 acidificating effect Effects 0.000 claims abstract description 10
- 238000011084 recovery Methods 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 62
- 239000007788 liquid Substances 0.000 claims description 44
- 238000002425 crystallisation Methods 0.000 claims description 35
- 230000008025 crystallization Effects 0.000 claims description 35
- 239000002994 raw material Substances 0.000 claims description 32
- 238000007789 sealing Methods 0.000 claims description 26
- 239000003513 alkali Substances 0.000 claims description 22
- 239000000498 cooling water Substances 0.000 claims description 20
- 239000012535 impurity Substances 0.000 claims description 20
- 238000009833 condensation Methods 0.000 claims description 12
- 230000005494 condensation Effects 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 9
- 238000001179 sorption measurement Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000001556 precipitation Methods 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 8
- 238000010926 purge Methods 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- 238000003860 storage Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 239000004519 grease Substances 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 230000020477 pH reduction Effects 0.000 claims description 6
- 239000000084 colloidal system Substances 0.000 claims description 5
- 239000008258 liquid foam Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 16
- 238000007670 refining Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 16
- 239000000243 solution Substances 0.000 description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000007789 gas Substances 0.000 description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000000855 fermentation Methods 0.000 description 6
- 230000004151 fermentation Effects 0.000 description 6
- 239000012141 concentrate Substances 0.000 description 5
- 239000002912 waste gas Substances 0.000 description 5
- 238000004061 bleaching Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000012452 mother liquor Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 3
- BDKLKNJTMLIAFE-UHFFFAOYSA-N 2-(3-fluorophenyl)-1,3-oxazole-4-carbaldehyde Chemical compound FC1=CC=CC(C=2OC=C(C=O)N=2)=C1 BDKLKNJTMLIAFE-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 235000021588 free fatty acids Nutrition 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- 229940087562 sodium acetate trihydrate Drugs 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 101100012902 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) FIG2 gene Proteins 0.000 description 1
- 101100233916 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) KAR5 gene Proteins 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000009874 alkali refining Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000003895 organic fertilizer Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- -1 sodium fatty acid Chemical class 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 230000002311 subsequent effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D9/00—Other inorganic fertilisers
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F17/00—Preparation of fertilisers characterised by biological or biochemical treatment steps, e.g. composting or fermentation
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/487—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/40—Bio-organic fraction processing; Production of fertilisers from the organic fraction of waste or refuse
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- Chemical & Material Sciences (AREA)
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- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Pest Control & Pesticides (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
- Molecular Biology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
Description
技术领域Technical Field
本发明属于油脂副产物精炼技术领域,尤其涉及一种在油脂副产物中醋酸钠的回收处理系统及工艺。The invention belongs to the technical field of oil by-product refining, and in particular relates to a system and process for recovering and treating sodium acetate in oil by-products.
背景技术Background Art
皂脚是粮油加工产业的副产物,是油脂精炼工段的碱炼脱酸步骤中形成的,该过程采用氢氧化钠中和毛油中的游离脂肪酸(FFA),所生成的皂吸附部分其他杂质从油中沉降分离,形成皂脚。皂脚的主要成分如下:脂肪酸钠、中性油、水其他杂质。Soapstock is a by-product of the grain and oil processing industry. It is formed in the alkali refining and deacidification step of the oil refining section. In this process, sodium hydroxide is used to neutralize the free fatty acids (FFA) in the crude oil. The generated soap absorbs some other impurities and precipitates and separates from the oil to form soapstock. The main components of soapstock are as follows: sodium fatty acid, neutral oil, water and other impurities.
目前,处理皂脚油脚有采用有机酸的创新工艺,例如用醋酸进行酸化,得到粗醋酸钠、脂肪酸、中性油等副产物。其中,醋酸钠是污水处理、食品行业、清洁剂的添加剂以及健康产业中不可或缺的化工原料,若对醋醋酸钠水溶液进行合理回收再利用具有很大的市场需求。At present, there are innovative processes using organic acids to treat soap stock, such as acidification with acetic acid to obtain by-products such as crude sodium acetate, fatty acids, neutral oils, etc. Among them, sodium acetate is an indispensable chemical raw material in sewage treatment, food industry, detergent additives and health industry. If the sodium acetate aqueous solution is reasonably recycled and reused, there will be a great market demand.
发明内容Summary of the invention
本发明的目的是提供一种在油脂副产物中醋酸钠的回收处理系统及工艺,通过本发明的系统及回收工艺,将粗醋酸钠水溶液中的油脂、酸性物质及油相进行有效脱除以后,将含水量在90%的醋酸钠水溶液经过三效蒸发器蒸发至结晶浓度,结晶产出三水醋酸钠,且用三效蒸发器比单效蒸发器节约能源70%左右。The purpose of the present invention is to provide a system and process for recovering and treating sodium acetate in oil by-products. Through the system and the recovery process of the present invention, after the oil, acidic substances and oil phase in the crude sodium acetate aqueous solution are effectively removed, the sodium acetate aqueous solution with a water content of 90% is evaporated to a crystallization concentration through a triple-effect evaporator, and sodium acetate trihydrate is produced by crystallization. The triple-effect evaporator saves about 70% of energy compared with the single-effect evaporator.
为达到上述目的,本发明采用的技术方案是:In order to achieve the above object, the technical solution adopted by the present invention is:
一种在油脂副产物中醋酸钠的回收处理系统,包括醋酸钠水溶液脱色工序、醋酸钠水溶液过滤、pH调节工序、醋酸钠水溶液蒸发工序。A sodium acetate recovery and treatment system in oil by-products comprises a sodium acetate aqueous solution decolorization process, a sodium acetate aqueous solution filtration process, a pH adjustment process, and a sodium acetate aqueous solution evaporation process.
进一步地,所述醋酸钠水溶液脱色工序包括将醋酸钠水溶液和活性炭进行混合的预混罐,与预混罐出口相连的脱色塔以及从脱色塔出口经离心泵抽出送至醋酸钠水溶液过滤及pH调节工序的原料。Furthermore, the sodium acetate aqueous solution decolorization process includes a premixing tank for mixing the sodium acetate aqueous solution and activated carbon, a decolorization tower connected to the outlet of the premixing tank, and raw materials pumped out from the outlet of the decolorization tower by a centrifugal pump and sent to the sodium acetate aqueous solution filtration and pH adjustment process.
进一步地,所述醋酸钠水溶液在进入预混罐之前需要和蒸汽在第一板式换热器内换热之后进入预混罐,所述脱色塔顶部设有液沫捕集器,脱色塔底部出液管原料分两路分别与4bar蒸汽换热以后经离心泵送往醋酸钠水溶液过滤及pH调节工序备用。Furthermore, the sodium acetate aqueous solution needs to be heat exchanged with steam in the first plate heat exchanger before entering the premixing tank. A liquid foam collector is provided on the top of the bleaching tower. The raw materials in the liquid outlet pipe at the bottom of the bleaching tower are divided into two paths and heat exchanged with 4bar steam respectively, and then sent to the sodium acetate aqueous solution filtration and pH adjustment process through a centrifugal pump for standby.
进一步地,所述醋酸钠水溶液过滤及pH调节工序包括叶片过滤机,叶片过滤机底部出口与蛟龙输送机相连,叶片过滤机上设有一个出料口和一个进料口,进料口位于叶片过滤机底部,叶片过滤机中部设有一个出料口直接将物料送往物料储罐,还包括碱液罐,碱液罐出口通过定量泵将碱液送入叶片过滤机出料口管道将醋酸钠水溶液的pH值进行调节。Furthermore, the sodium acetate aqueous solution filtration and pH adjustment process includes a blade filter, the bottom outlet of the blade filter is connected to the Jiaolong conveyor, and the blade filter is provided with a discharge port and a feed port. The feed port is located at the bottom of the blade filter, and a discharge port is provided in the middle of the blade filter to directly send the material to the material storage tank. It also includes an alkali liquid tank, and the alkali liquid outlet of the alkali liquid tank is sent into the blade filter discharge port pipeline through a metering pump to adjust the pH value of the sodium acetate aqueous solution.
进一步地,所述叶片过滤机上部还设有一个出口管路,该出口管路上设有一个吹扫管路,所述吹扫管路与4bar的饱和蒸汽管道相连通,所述出口管路末端设有水汽分离器,水汽分离器底部设有液体出口,液体出口与浊水罐相连,水汽分离器上部设有气体出口,气体出口端部设有吹饼冷凝器,所述浊水罐出口通过离心泵将物料送入醋酸钠脱色工段中的脱色罐中进一步脱色,所述叶片过滤机进料口和出料口管路上均设有旁路,旁路均与浊水罐相连通,所述叶片过滤机还设有一个空气进口,所述空气进口与6bar的压缩空气管道相连通,所述叶片过滤机为两个,两个叶片过滤机并联设置,还包括滤板洗涤池。Furthermore, an outlet pipeline is provided on the upper part of the blade filter, and a purge pipeline is provided on the outlet pipeline, and the purge pipeline is connected to a 4bar saturated steam pipeline. A water vapor separator is provided at the end of the outlet pipeline, and a liquid outlet is provided at the bottom of the water vapor separator, and the liquid outlet is connected to a turbid water tank. A gas outlet is provided on the upper part of the water vapor separator, and a cake blowing condenser is provided at the end of the gas outlet. The outlet of the turbid water tank sends the material to the decolorization tank in the sodium acetate decolorization section through a centrifugal pump for further decolorization. The feed port and the discharge port pipeline of the blade filter are both provided with bypasses, and the bypasses are both connected to the turbid water tank. The blade filter is also provided with an air inlet, and the air inlet is connected to a 6bar compressed air pipeline. There are two blade filters, and the two blade filters are arranged in parallel, and also include a filter plate washing tank.
进一步地,醋酸钠水溶液蒸发工序包括将原料进入进料罐以后通过三效进料泵送入第二板式换热器换热以后再送入三效分离器经底部出口管道流入三效加热器,三效加热器经其底部的二效进料泵送入二效分离器中,二效分离器原料经其底部管道流入二效加热器,二效加热器经一效进料泵流入一效分离器内,一效分离器经其底部出料管和一效循环泵送入一效加热器内,产生的气体送入一效分离器继续分离,当原料浓度达到一定值时,打开一效出料泵,将原料送往结晶罐结晶,将结晶完成的原料送入离心机分离,从离心机出来的固体送去产品工段包装,液体送入缓冲罐暂存,通过泵送往脱色工段再次进入过滤并参与再次结晶。Furthermore, the sodium acetate aqueous solution evaporation process includes that after the raw material enters the feed tank, it is sent to the second plate heat exchanger through the triple-effect feed pump for heat exchange, and then sent to the triple-effect separator through the bottom outlet pipe to flow into the triple-effect heater, the triple-effect heater is sent to the second-effect separator through the second-effect feed pump at the bottom, the raw material of the second-effect separator flows into the second-effect heater through its bottom pipe, the second-effect heater flows into the first-effect separator through the first-effect feed pump, the first-effect separator is sent into the first-effect heater through its bottom discharge pipe and the first-effect circulation pump, the generated gas is sent to the first-effect separator for further separation, when the raw material concentration reaches a certain value, the first-effect discharge pump is turned on, the raw material is sent to the crystallization tank for crystallization, the crystallized raw material is sent to the centrifuge for separation, the solid coming out of the centrifuge is sent to the product section for packaging, the liquid is sent to the buffer tank for temporary storage, and is sent to the decolorization section by a pump to enter the filtration again and participate in the crystallization again.
进一步地,所述缓冲罐设有缓冲泵,缓冲泵将缓冲液送入其他工段或外排,还包括机封水罐,所述机封水罐通过密封水泵将冷却水分别送入缓冲泵、一效出料泵、一效循环泵、一效进料泵、二效进料泵、三效进料泵冷却后经回收管道回流进机封水罐再次利用,还包括表面冷凝器,表面冷凝器的热源来自三效分离器分离的蒸汽,表面冷凝器上设有冷却水进口和冷却水出口,表面冷凝器底部的出水管道与表冷水封罐联通,所述一效加热器、二效加热器和三效加热器内的冷凝液均与表冷水封罐相连通,且表冷水封罐内的水一部分与三效分离器顶部的热蒸汽混合进入表面冷凝器进一步利用,表冷水封罐另一部分水经冷凝水泵送入冷凝水罐作为第二板式换热器的冷源使用,表面冷凝器底部设有一个真空泵,所述冷凝水泵的冷却水进口与密封水泵出水口相连,冷凝水泵出口与机封水罐相连,所述一效加热器还设有加热蒸汽进口,一效分离器顶部的蒸汽通道与二效加热器相连,二效分离器顶部的蒸汽通道与三效加热器相连。Furthermore, the buffer tank is provided with a buffer pump, which delivers the buffer to other work sections or discharges it externally. It also includes a machine sealing water tank, which delivers cooling water to the buffer pump, the first-effect discharge pump, the first-effect circulation pump, the first-effect feed pump, the second-effect feed pump, and the third-effect feed pump respectively through a sealing water pump. After cooling, the cooling water flows back into the machine sealing water tank through a recovery pipeline for reuse. It also includes a surface condenser. The heat source of the surface condenser comes from the steam separated by the three-effect separator. A cooling water inlet and a cooling water outlet are provided on the surface condenser. The outlet pipe at the bottom of the surface condenser is connected to the surface cold water sealing tank. The first-effect heater, the second-effect heater and the three-effect heater The condensate in the device is connected with the surface cooling water sealing tank, and part of the water in the surface cooling water sealing tank is mixed with the hot steam at the top of the three-effect separator and enters the surface condenser for further utilization. Another part of the water in the surface cooling water sealing tank is sent to the condensation water tank through the condensation water pump and used as the cold source of the second plate heat exchanger. A vacuum pump is provided at the bottom of the surface condenser, the cooling water inlet of the condensation water pump is connected with the water outlet of the sealing water pump, and the outlet of the condensation water pump is connected with the machine sealing water tank. The first-effect heater is also provided with a heating steam inlet, the steam channel at the top of the first-effect separator is connected with the second-effect heater, and the steam channel at the top of the second-effect separator is connected with the three-effect heater.
进一步地,所述醋酸钠水溶液在进入预混罐之前,先经过沉淀和除杂工序,除去醋酸钠水溶液的杂质,除杂后的醋酸钠水溶液通过第一板式换热器换热后进入预混罐。Furthermore, before entering the premixing tank, the sodium acetate aqueous solution is first subjected to a precipitation and impurity removal process to remove impurities in the sodium acetate aqueous solution. The sodium acetate aqueous solution after impurity removal passes through a first plate heat exchanger and then enters the premixing tank.
本发明还提供了一种利用上述系统进行醋酸钠回收处理的工艺,所述工艺包括以下步骤:The present invention also provides a process for recovering sodium acetate using the above system, the process comprising the following steps:
1)将来自酸化工段的粗的醋酸钠水溶液送入醋酸钠水溶液脱色工序,通过活性炭的吸附作用将其含有的油脂和胶质物及酸性物质进行脱除;1) The crude sodium acetate aqueous solution from the acidification section is sent to the sodium acetate aqueous solution decolorization process, and the grease, colloid and acidic substances contained therein are removed by the adsorption of activated carbon;
2)将来自步骤1)中经过脱色处理的醋酸钠水溶液与活性炭的混合液送入醋酸钠水溶液过滤及pH调节工序经过叶片过滤机的过滤处理以后再将pH值调整至7以后得到中性的醋酸钠水溶液;2) sending the mixed solution of the sodium acetate aqueous solution and activated carbon which has been decolorized in step 1) to a sodium acetate aqueous solution filtration and pH adjustment process, filtering it through a leaf filter, and then adjusting the pH value to 7 to obtain a neutral sodium acetate aqueous solution;
3)将来自步骤2)中的醋酸钠水溶液送入醋酸钠水溶液蒸发工序进行蒸发结晶处理即可得到水分含量在5%的醋酸钠晶体。3) The sodium acetate aqueous solution from step 2) is sent to the sodium acetate aqueous solution evaporation process for evaporation and crystallization to obtain sodium acetate crystals with a water content of 5%.
进一步地,在步骤1)中,在进行活性炭吸附之前,先将粗醋酸钠水溶液pH调节至6-9,调节时控制温度为60-70℃。Furthermore, in step 1), before the activated carbon adsorption, the pH of the crude sodium acetate aqueous solution is adjusted to 6-9, and the temperature is controlled to 60-70°C during the adjustment.
进一步地,在步骤1)中,所述活性炭的加入量为醋酸钠水溶液量的1-10%,脱色时间为1-2h。Furthermore, in step 1), the amount of activated carbon added is 1-10% of the amount of the sodium acetate aqueous solution, and the decolorization time is 1-2 hours.
进一步地,在步骤2)中,经叶片过滤机处理过以后的固体活性炭送去发酵塔发酵,发酵后最终作为肥料混合外售。Furthermore, in step 2), the solid activated carbon treated by the leaf filter is sent to a fermentation tower for fermentation, and after fermentation, it is finally mixed and sold as a fertilizer.
进一步地,在步骤3)中,所述蒸发采用三效蒸发器蒸发,控制三效蒸发的真空度为90-100pa、二效蒸发的真空度为70-80pa、一效蒸发的真空度为40-50pa,所述一效蒸发温度为75-80℃,蒸发好的所述醋酸钠浓缩液为25-35°Bé。Furthermore, in step 3), the evaporation is carried out by a triple-effect evaporator, the vacuum degree of the triple-effect evaporation is controlled to be 90-100 Pa, the vacuum degree of the second-effect evaporation is controlled to be 70-80 Pa, the vacuum degree of the first-effect evaporation is controlled to be 40-50 Pa, the first-effect evaporation temperature is 75-80° C., and the evaporated sodium acetate concentrate is 25-35° Bé.
进一步地,在步骤3)中,所述结晶温度为55-60℃,结晶时间为4-48h。Furthermore, in step 3), the crystallization temperature is 55-60° C., and the crystallization time is 4-48 hours.
进一步地,将步骤3)中结晶完成的料液,进行离心分离、甩干,即得到含水5%以内的三水醋酸钠,得到的母液再次回收利用,所述离心转速为1400-1900rpm。Furthermore, the crystallized liquid in step 3) is centrifuged and dried to obtain sodium acetate trihydrate with a water content of less than 5%, and the obtained mother liquor is recycled again, and the centrifugal speed is 1400-1900rpm.
综上所述,由于本发明采用了上述技术方案,本发明具有以下有益效果:In summary, since the present invention adopts the above technical solution, the present invention has the following beneficial effects:
1、粗醋酸钠水溶液经醋酸钠水溶液脱色工序以后将粗醋酸钠水溶液中的油相、酸性物质及杂质负载于活性炭上,使醋酸钠水溶液进一步净化为后续的蒸发提供有力的帮助,且吸附有油相、酸性物质及杂质的活性炭可以送至发酵工段发酵作为有机肥继续使用,没有废弃物的产生,对环境友好。1. After the crude sodium acetate aqueous solution is decolorized by the sodium acetate aqueous solution, the oil phase, acidic substances and impurities in the crude sodium acetate aqueous solution are loaded on the activated carbon, so that the sodium acetate aqueous solution is further purified to provide a strong help for the subsequent evaporation, and the activated carbon adsorbed with the oil phase, acidic substances and impurities can be sent to the fermentation section for fermentation and continued to be used as an organic fertilizer, without the generation of waste, which is environmentally friendly.
2、醋酸钠水溶液过滤及pH调节工序的设置将来自上一工段即醋酸钠水溶液脱色工段中的醋酸钠水溶液经过叶片过滤机的进一步分离,又通过碱液罐的调节,使得后续在制备醋酸钠晶体时得到的纯净度更高,增加了其附加价值,叶片过滤机设置的与6bar的压缩蒸汽管道相连通的气路确保过滤片上的固体物质能够被顺利吹扫下来防止堵塞,从叶片过滤机处出来的醋酸钠溶液经碱液罐内碱液的调节以便于后期蒸发工序的处理,整个装置衔接紧密,使用方便;2. Setting of the sodium acetate aqueous solution filtration and pH adjustment process: The sodium acetate aqueous solution from the previous process, i.e., the sodium acetate aqueous solution decolorization process, is further separated by the leaf filter, and then adjusted by the alkali liquid tank, so that the purity obtained in the subsequent preparation of sodium acetate crystals is higher, which increases its added value. The air path connected to the 6bar compressed steam pipeline provided by the leaf filter ensures that the solid matter on the filter plate can be smoothly blown down to prevent clogging. The sodium acetate solution coming out of the leaf filter is adjusted by the alkali liquid in the alkali liquid tank to facilitate the treatment of the later evaporation process. The whole device is tightly connected and easy to use.
3、采用三效蒸发器对醋酸钠水溶液进行蒸发结晶,三效蒸发原理是由三个蒸发器组合后的蒸发操作,三效蒸发器在运行时,需要后效的压强和溶液的沸点均低于前效蒸发器,引入前效的二次蒸汽作为后效的加热介质,即后效的加热室成为前效二次蒸汽的冷凝器,第一效需要消耗生锅炉蒸汽,三效蒸发比单效蒸发器节约能源70%左右,另外本申请中三效分离器最终的蒸汽去往表面冷凝器冷凝,冷凝下来的带有一定温度的液体送入表冷水封罐继续与三效分离器的蒸汽混合,一方面减少了表面冷凝器的工作负荷,另一方面将整个系统的余热进行回收再利用,充分利用了整个系统的热量,减少热量损失;3. A triple-effect evaporator is used to evaporate and crystallize the sodium acetate aqueous solution. The principle of triple-effect evaporation is an evaporation operation after the combination of three evaporators. When the triple-effect evaporator is in operation, the pressure of the after-effect and the boiling point of the solution are required to be lower than those of the front-effect evaporator. The secondary steam of the front-effect is introduced as the heating medium of the after-effect, that is, the heating chamber of the after-effect becomes the condenser of the secondary steam of the front-effect. The first effect needs to consume the steam of the boiler. The triple-effect evaporation saves about 70% of energy compared with the single-effect evaporator. In addition, the final steam of the triple-effect separator in this application goes to the surface condenser for condensation, and the condensed liquid with a certain temperature is sent to the surface cold water sealing tank to continue to mix with the steam of the triple-effect separator. On the one hand, the workload of the surface condenser is reduced, and on the other hand, the waste heat of the entire system is recycled and reused, which makes full use of the heat of the entire system and reduces heat loss.
4、本发明通过各个工序的有效衔接处理,使得最终得到的醋酸钠成品的纯度得到很大提升,含水量从90%降至5%,有效解决了油脂副产物加工过程中,钠盐的资源化利用的问题;4. The present invention effectively connects various processes, so that the purity of the final sodium acetate product is greatly improved, and the water content is reduced from 90% to 5%, which effectively solves the problem of resource utilization of sodium salt in the processing of oil by-products;
5、本发明的粗醋酸钠水溶液在进入预混罐之前,先进行沉淀和除杂工序,在进行活性炭脱色前除去粗醋酸钠中的固体杂质,进一步提升了粗醋酸钠溶液的脱色效果。5. The crude sodium acetate aqueous solution of the present invention is first subjected to a precipitation and impurity removal process before entering the premixing tank, and solid impurities in the crude sodium acetate are removed before the activated carbon decolorization, thereby further improving the decolorization effect of the crude sodium acetate solution.
6、本发明的粗醋酸钠水溶液在进行活性炭脱色前,先将粗醋酸钠水溶液的pH调节至6-9,在此pH条件下加入活性炭对粗醋酸钠中含有的油相、酸性物质及杂质吸附脱除,使得粗醋酸钠的脱色效果大大提高;同时使得醋酸钠水溶液蒸发工序将蒸发产生的冷凝水COD控制在300-450mg/L,大大的降低了对环境的污染。6. Before the crude sodium acetate aqueous solution of the present invention is subjected to activated carbon decolorization, the pH of the crude sodium acetate aqueous solution is first adjusted to 6-9, and activated carbon is added under this pH condition to adsorb and remove the oil phase, acidic substances and impurities contained in the crude sodium acetate, so that the decolorization effect of the crude sodium acetate is greatly improved; at the same time, the evaporation process of the sodium acetate aqueous solution controls the COD of the condensed water generated by evaporation to 300-450 mg/L, thereby greatly reducing the pollution to the environment.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
图1是本发明中醋酸钠水溶液脱色工序的结构示意图;Fig. 1 is a schematic structural diagram of a sodium acetate aqueous solution decolorization process in the present invention;
图2是本发明中醋酸钠水溶液过滤及PH调节工序的结构示意图;FIG2 is a schematic structural diagram of the sodium acetate aqueous solution filtration and pH adjustment process in the present invention;
图3是本发明中醋酸钠水溶液蒸发工序的结构示意图;FIG3 is a schematic structural diagram of the evaporation process of the sodium acetate aqueous solution in the present invention;
图4是本发明一种在油脂副产物中醋酸钠的回收处理系统的结构简图。FIG. 4 is a schematic structural diagram of a system for recovering and treating sodium acetate in oil by-products according to the present invention.
具体实施方式DETAILED DESCRIPTION
为使本发明的目的、技术方案及优点更加清楚明白,下面举出优选实施例,对本发明进一步详细说明。然而,需要说明的是,说明书中列出的许多细节仅仅是为了使读者对本发明的一个或多个方面有一个透彻的理解,即便没有这些特定的细节也可以实现本发明的这些方面。In order to make the purpose, technical solution and advantages of the present invention more clearly understood, preferred embodiments are given below to further describe the present invention in detail. However, it should be noted that many details listed in the specification are only for the purpose of enabling the reader to have a thorough understanding of one or more aspects of the present invention, and these aspects of the present invention can be implemented even without these specific details.
实施例1Example 1
如图1-图4所示,一种在油脂副产物中醋酸钠的回收处理系统,包括醋酸钠水溶液脱色工序、醋酸钠水溶液过滤及pH调节工序以及醋酸钠水溶液蒸发工序,醋酸钠水溶液脱色工序包括将醋酸钠水溶液和活性炭进行混合的预混罐111,与预混罐111出口相连的脱色塔112以及从脱色塔112出口经离心泵113抽出送至醋酸钠水溶液过滤及pH调节工序的原料,该pH调节工序采用在线pH传感器在线自动调节,可达到连续进料处理的效果。醋酸钠水溶液在进入预混罐111之前需要和蒸汽在第一板式换热器114内换热之后进入预混罐111,脱色塔112顶部设有液沫捕集器115,用于捕集罐内液沫和挥发的醋酸废气,并将废气冷凝后,送尾气处理系统处理,该脱色过程为1-2小时,脱色塔112底部出液管原料分两路分别与4bar蒸汽换热以后经离心泵113送往醋酸钠水溶液过滤及pH调节工序备用。As shown in Figures 1 to 4, a sodium acetate recovery and treatment system in oil by-products includes a sodium acetate aqueous solution decolorization process, a sodium acetate aqueous solution filtration and pH adjustment process, and a sodium acetate aqueous solution evaporation process. The sodium acetate aqueous solution decolorization process includes a premixing tank 111 for mixing the sodium acetate aqueous solution and activated carbon, a decolorization tower 112 connected to the outlet of the premixing tank 111, and raw materials pumped out from the outlet of the decolorization tower 112 through a centrifugal pump 113 and sent to the sodium acetate aqueous solution filtration and pH adjustment process. The pH adjustment process adopts an online pH sensor for online automatic adjustment, which can achieve the effect of continuous feeding processing. Before entering the premixing tank 111, the sodium acetate aqueous solution needs to exchange heat with steam in the first plate heat exchanger 114 and then enter the premixing tank 111. A liquid foam collector 115 is provided on the top of the bleaching tower 112 to collect the liquid foam and volatilized acetic acid waste gas in the tank, and condense the waste gas before sending it to the tail gas treatment system for treatment. The decolorization process takes 1-2 hours. The raw materials at the bottom of the liquid outlet pipe of the bleaching tower 112 are divided into two paths and exchanged with 4bar steam respectively, and then sent to the sodium acetate aqueous solution filtration and pH adjustment process through a centrifugal pump 113 for standby.
醋酸钠水溶液在进入预混罐111之前,先经过沉淀和除杂工序,除去醋酸钠水溶液的杂质,除杂后的醋酸钠水溶液通过第一板式换热器114换热后进入预混罐111。在本发明中,粗醋酸钠水溶液在进行活性炭脱色处理前先进入沉淀罐117沉淀,沉淀完成后再进入除杂罐118进行除杂,沉淀除杂完成后的粗醋酸钠水溶液再通过第一板式换热器114进行换热后进入预混罐111,再进行接下来的活性炭脱色等处理工序。Before entering the premixing tank 111, the sodium acetate aqueous solution first undergoes a precipitation and impurity removal process to remove impurities in the sodium acetate aqueous solution. The sodium acetate aqueous solution after impurity removal passes through the first plate heat exchanger 114 and then enters the premixing tank 111. In the present invention, the crude sodium acetate aqueous solution first enters the precipitation tank 117 for precipitation before the activated carbon decolorization treatment, and then enters the impurity removal tank 118 for impurity removal after the precipitation is completed. After the precipitation and impurity removal, the crude sodium acetate aqueous solution passes through the first plate heat exchanger 114 for heat exchange and then enters the premixing tank 111, and then undergoes the subsequent activated carbon decolorization and other treatment processes.
醋酸钠水溶液过滤及pH调节工序包括叶片过滤机121,叶片过滤机121底部出口与蛟龙输送机相连,从叶片过滤机121出口的固体物料被送往微生物发酵罐进行生物堆肥,叶片过滤机121上设有一个出料口122和一个进料口123,进料口123位于叶片过滤机121底部,叶片过滤机121中部设有一个出料口122直接将物料送往物料储罐124,还包括碱液罐125,碱液罐125出口通过定量泵126将碱液送入叶片过滤机121出料口管道将醋酸钠水溶液的pH值进行调节,叶片过滤机121上部还设有一个出口管路127,该出口管路127上设有一个吹扫管路,吹扫管路128与4bar的饱和蒸汽管道相连通,吹扫管路128用于将叶片过滤机121内部的气液混合物送入水气分离器129进一步分离,出口管路127末端设有水汽分离器129,水汽分离器129底部设有液体出口,液体出口与浊水罐1210相连,水汽分离器129上部设有气体出口,气体出口端部设有吹饼冷凝器1211,浊水罐1210出口通过离心泵将物料送入醋酸钠脱色工段中的脱色罐中进一步脱色,叶片过滤机121进料口和出料口管路上均设有旁路,旁路均与浊水罐1210相连通,叶片过滤机121还设有一个空气进口,空气进口与6bar的压缩蒸汽管道相连通,叶片过滤机121为两个,两个叶片过滤机121并联设置,碱液罐125出口管路还设有一个备用定量泵126,用于设备出现故障时备用,还包括滤板洗涤池1212,用于清洗本装置的叶片过滤机121的滤板,设置将来自上一工段即醋酸钠水溶液脱色工段中的醋酸钠水溶液经过叶片过滤机的进一步分离,又通过碱液罐125的调节,使得后续在制备醋酸钠晶体时得到的纯净度更高,增加了其附加价值,叶片过滤机设置的与6bar的压缩蒸汽管道相连通的气路确保过滤片上的固体物质能够被顺利吹扫下来防止堵塞,从叶片过滤机处出来的醋酸钠溶液经碱液罐内碱液的调节以便于后期蒸发工序的处理,整个装置衔接紧密,使用方便。The sodium acetate aqueous solution filtration and pH adjustment process includes a blade filter 121, the bottom outlet of the blade filter 121 is connected to the Jiaolong conveyor, and the solid material from the outlet of the blade filter 121 is sent to the microbial fermentation tank for biocomposting. The blade filter 121 is provided with a discharge port 122 and a feed port 123, and the feed port 123 is located at the bottom of the blade filter 121. The blade filter 121 is provided with a discharge port 122 in the middle to directly send the material to the material storage tank 124, and also includes an alkali liquid tank 125. The outlet of the alkali liquid tank 125 sends the alkali liquid into the blade filter 121 through a metering pump 126 for discharge. The pH value of the sodium acetate aqueous solution is adjusted by an inlet pipe. An outlet pipe 127 is also provided on the upper part of the leaf filter 121. A purge pipe is provided on the outlet pipe 127. The purge pipe 128 is connected to a 4 bar saturated steam pipe. The purge pipe 128 is used to send the gas-liquid mixture inside the leaf filter 121 to a water-gas separator 129 for further separation. A water-gas separator 129 is provided at the end of the outlet pipe 127. A liquid outlet is provided at the bottom of the water-gas separator 129. The liquid outlet is connected to the turbid water tank 1210. A gas outlet is provided on the upper part of the water-gas separator 129. A purge pipe is provided at the end of the gas outlet. Condenser 1211, the outlet of the turbid water tank 1210 is used to send the material to the decolorization tank in the sodium acetate decolorization section for further decolorization through a centrifugal pump. The feed port and the discharge port pipeline of the blade filter 121 are both provided with bypasses, which are both connected to the turbid water tank 1210. The blade filter 121 is also provided with an air inlet, which is connected to a 6 bar compressed steam pipeline. There are two blade filters 121, which are arranged in parallel. The outlet pipeline of the alkali liquid tank 125 is also provided with a spare quantitative pump 126 for standby use when the equipment fails. It also includes a filter plate washing tank 1212 for cleaning the filter plate. The filter plate of the blade filter 121 of the device is arranged to further separate the sodium acetate aqueous solution from the previous process section, i.e., the sodium acetate aqueous solution decolorization process section, through the blade filter, and then through the regulation of the alkali liquid tank 125, so that the purity obtained in the subsequent preparation of sodium acetate crystals is higher, thereby increasing its added value. The air path connected to the 6 bar compressed steam pipeline provided in the blade filter ensures that the solid matter on the filter plate can be smoothly blown down to prevent clogging. The sodium acetate solution coming out of the blade filter is regulated by the alkali liquid in the alkali liquid tank to facilitate the processing of the subsequent evaporation process. The whole device is tightly connected and easy to use.
醋酸钠水溶液过滤及pH调节工序还包括袋式过滤器130,袋式过滤器130的进料口与叶片过滤机121的出料口122连接,所述袋式过滤器130的出料口与物料储罐124连接,所述碱液罐125的碱液出料口通过定量泵126将碱液送入物料储罐124将醋酸钠水溶液的pH值进行调节。The sodium acetate aqueous solution filtration and pH adjustment process also includes a bag filter 130, the feed port of the bag filter 130 is connected to the discharge port 122 of the blade filter 121, the discharge port of the bag filter 130 is connected to the material storage tank 124, and the alkali liquid discharge port of the alkali liquid tank 125 sends the alkali liquid into the material storage tank 124 through the metering pump 126 to adjust the pH value of the sodium acetate aqueous solution.
醋酸钠水溶液蒸发工序在设备没有运行时,先将原料进入进料罐131以后通过三效进料泵132送入第二板式换热器133换热以后再送入三效分离器4经底部出口管道流入三效加热器135,三效加热器135经其底部的二效进料泵136送入二效分离器137中,二效分离器137原料经其底部管道流入二效加热器8,二效加热器138经一效进料泵139流入一效分离器1310内,一效分离器1310经其底部出料管和一效循环泵1311送入一效加热器1312内,产生的气体送入一效分离器1310继续分离,当原料浓度达到一定值时,打开一效出料泵,将原料送往结晶罐结晶,将结晶完成的原料送入离心机1315分离,从离心机1315出来的固体送去产品工段包装,液体送入缓冲罐1316暂存,通过泵送往脱色工段再次进入过滤并参与再次结晶。结晶罐有多个,采用多罐并联模式,可满足多批原料浓缩液同时进行结晶操作,提高了本发明系统的生产效率,该结晶罐内含锚式搅拌桨,罐体内壁为搪瓷材质,可减少醋酸钠晶体的粘壁现象,提高产品得率,结晶罐设置自动控制降温速率,通过调节降温速率及搅拌速度,结晶时间根据浓缩液的状况和结晶曲线,控制在4-48小时,结晶结束后通过送料泵送到离心机分离,罐体内还设置有温度传感器,用于监控结晶冷却曲线。In the sodium acetate aqueous solution evaporation process, when the equipment is not running, the raw material first enters the feed tank 131 and is then sent to the second plate heat exchanger 133 through the triple-effect feed pump 132 for heat exchange, and then sent to the triple-effect separator 4 through the bottom outlet pipe to flow into the triple-effect heater 135. The triple-effect heater 135 is sent to the second-effect separator 137 through the second-effect feed pump 136 at the bottom. The raw material of the second-effect separator 137 flows into the second-effect heater 8 through the bottom pipe. The second-effect heater 138 flows into the first-effect separator 1310 through the first-effect feed pump 139. The first-effect separator 1310 is fed into the first-effect heater 1312 through the bottom discharge pipe and the first-effect circulation pump 1311, and the generated gas is fed into the first-effect separator 1310 for further separation. When the raw material concentration reaches a certain value, the first-effect discharge pump is turned on to send the raw material to the crystallization tank for crystallization, and the crystallized raw material is sent to the centrifuge 1315 for separation. The solid coming out of the centrifuge 1315 is sent to the product section for packaging, and the liquid is sent to the buffer tank 1316 for temporary storage, and then sent to the decolorization section by a pump to enter the filtration again and participate in crystallization again. There are multiple crystallization tanks, which adopt a multi-tank parallel mode, which can meet the crystallization operation of multiple batches of raw material concentrates at the same time, thereby improving the production efficiency of the system of the present invention. The crystallization tank contains an anchor-type stirring paddle, and the inner wall of the tank is made of enamel material, which can reduce the wall adhesion phenomenon of sodium acetate crystals and improve the product yield. The crystallization tank is set to automatically control the cooling rate. By adjusting the cooling rate and the stirring speed, the crystallization time is controlled within 4-48 hours according to the condition of the concentrated liquid and the crystallization curve. After the crystallization is completed, it is sent to a centrifuge for separation through a feeding pump. A temperature sensor is also arranged in the tank body for monitoring the crystallization cooling curve.
缓冲罐1316设有缓冲泵,缓冲泵1317将缓冲液送入其他工段或外排,还包括机封水罐1318,机封水罐1318通过密封水泵1319将冷却水分别送入缓冲泵1317、一效出料泵1313、一效循环泵1311、一效进料泵139、二效进料泵136、三效进料泵132冷却后经回收管道回流进机封水罐1318再次利用,缓冲泵1317、一效出料泵1313、一效循环泵1311、一效进料泵139、二效进料泵136、三效进料泵132均属于高温泵,其长时间使用过后需要降温处理,还包括表面冷凝器1320,表面冷凝器1320的热源来自三效分离器134分离的蒸汽,表面冷凝器1320上设有冷却水进口和冷却水出口,表面冷凝器1320底部的出水管道与表冷水封罐1321联通,一效加热器1312、二效加热器138和三效加热器135内的冷凝液均与表冷水封罐1321相连通,且表冷水封罐1321内的水一部分与三效分离器4顶部的热蒸汽混合进入表面冷凝器1320进一步利用,表冷水封罐1321另一部分水经冷凝水泵1322送入冷凝水罐1323作为第二板式换热器133的冷源使用,表面冷凝器1320底部设有一个真空泵1324,真空泵1324用于调节整个系统的真空度,冷凝水泵1322的冷却水进口与密封水泵1319出水口相连,冷凝水泵1322出口与机封水罐1318相连,一效加热器1312还设有加热蒸汽进口,一效分离器1310顶部的蒸汽通道与二效加热器138相连,二效分离器137顶部的蒸汽通道与三效加热器135相连,这样设置可以充分利用前效的蒸汽作为后效的加热介质,对热量充分利用,具体使用时,一效加热器通过通入的高温蒸汽将介质加热,一部分液体蒸发后液位降低,且由于成品的排出液位进一步降低当降低到设定的高度时一效分离器将原料通过一效循环泵送入一效加热器继续反应,而后续的二效加热器进一步将原料通过一效进料泵送入一效分离器,二效分离器将原料送入二效加热器,从而三效加热器通过二效进料泵将原料送入二效分离器,三效分离器进一步将原料补充入三效加热器,从而进料罐通过三效进料泵将原料送入三效分离器中,逐层递补原料,原料在后效加热器中初步加热,减轻前效加热器的工作负担,且三效蒸发原理是由三个蒸发器组合后的蒸发操作,三效蒸发器在运行时,需要后效的压强和溶液的沸点均低于前效蒸发器,引入前效的二次蒸汽作为后效的加热介质,即后效的加热室成为前效二次蒸汽的冷凝器,第一效需要消耗生锅炉蒸汽,三效蒸发比单效蒸发器节约能源70%左右。The buffer tank 1316 is provided with a buffer pump, and the buffer pump 1317 sends the buffer to other sections or discharges it. It also includes a machine sealing water tank 1318. The machine sealing water tank 1318 sends cooling water to the buffer pump 1317, the first-effect discharge pump 1313, the first-effect circulation pump 1311, the first-effect feed pump 139, the second-effect feed pump 136, and the third-effect feed pump 132 through the sealing water pump 1319. After cooling, it flows back into the machine sealing water tank 1318 through the recovery pipeline for reuse. The buffer pump 1317, the first-effect discharge pump 1313, the first-effect circulation pump 1311, the first-effect feed pump 139, the second-effect feed pump 136, and the third-effect feed pump 132 are all high-temperature pumps, which need to be cooled after long-term use. It also includes a surface condenser 1320. The heat source of the surface condenser 1320 comes from the three-effect separator 134 is separated from the steam, and the surface condenser 1320 is provided with a cooling water inlet and a cooling water outlet. The water outlet pipe at the bottom of the surface condenser 1320 is connected to the surface cold water sealing tank 1321. The condensate in the first effect heater 1312, the second effect heater 138 and the third effect heater 135 are all connected to the surface cold water sealing tank 1321, and a part of the water in the surface cold water sealing tank 1321 is mixed with the hot steam at the top of the three-effect separator 4 and enters the surface condenser 1320 for further use. Another part of the water in the surface cold water sealing tank 1321 is sent to the condensation water tank 1323 through the condensation water pump 1322 as the cold source of the second plate heat exchanger 133. A vacuum pump 1324 is provided at the bottom of the surface condenser 1320. The vacuum pump 1324 is used to adjust the vacuum degree of the entire system. The condensation water pump 1322 The cooling water inlet is connected to the outlet of the sealing water pump 1319, the outlet of the condensing water pump 1322 is connected to the machine sealing water tank 1318, the first-effect heater 1312 is also provided with a heating steam inlet, the steam channel at the top of the first-effect separator 1310 is connected to the second-effect heater 138, and the steam channel at the top of the second-effect separator 137 is connected to the triple-effect heater 135. This arrangement can make full use of the steam of the previous effect as the heating medium of the subsequent effect, and make full use of the heat. When used specifically, the first-effect heater heats the medium by passing in high-temperature steam, and the liquid level decreases after a part of the liquid evaporates, and the discharge liquid level of the finished product is further reduced. When it is reduced to a set height, the first-effect separator sends the raw materials into the first-effect heater through the first-effect circulation pump for continued reaction, and the subsequent second-effect heater further sends the raw materials through The first-effect feed pump feeds the first-effect separator, and the second-effect separator feeds the raw materials into the second-effect heater, so that the three-effect heater feeds the raw materials into the second-effect separator through the second-effect feed pump, and the three-effect separator further replenishes the raw materials into the three-effect heater, so that the feed tank feeds the raw materials into the three-effect separator through the three-effect feed pump, and the raw materials are replenished layer by layer. The raw materials are preliminarily heated in the after-effect heater to reduce the workload of the front-effect heater. The principle of three-effect evaporation is an evaporation operation after the combination of three evaporators. When the three-effect evaporator is in operation, the pressure of the after-effect and the boiling point of the solution are required to be lower than those of the front-effect evaporator. The secondary steam of the front effect is introduced as the heating medium of the after-effect, that is, the heating chamber of the after-effect becomes the condenser of the secondary steam of the front effect. The first effect needs to consume the steam from the live boiler. The three-effect evaporation saves about 70% of energy compared with the single-effect evaporator.
实施例2Example 2
本实施例提供了一种利用实施例1的系统进行醋酸钠回收处理的工艺,该工艺包括以下步骤:This embodiment provides a process for recovering sodium acetate using the system of embodiment 1, and the process comprises the following steps:
1)将来自酸化工段的粗醋酸钠水溶液,先加入浓度为50%的液碱调节pH,将pH值调整为6,温度控制在60℃;将得到的pH值为6的粗醋酸钠水溶液送入醋酸钠水溶液脱色工序,加入活性炭进行脱色,活性炭的加入量为醋酸钠水溶液量的1%,脱色时间为2h,活性炭的吸附作用可将粗醋酸钠溶液中含有的油脂和胶质物及酸性物质进行脱除,得到原料混合液;1) Adding 50% liquid caustic soda to adjust the pH of the crude sodium acetate aqueous solution from the acidification section to adjust the pH value to 6, and controlling the temperature at 60° C. Sending the obtained crude sodium acetate aqueous solution with a pH value of 6 to a sodium acetate aqueous solution decolorization process, adding activated carbon for decolorization, the amount of activated carbon added is 1% of the amount of the sodium acetate aqueous solution, and the decolorization time is 2 hours. The adsorption of the activated carbon can remove the grease, colloid and acidic substances contained in the crude sodium acetate solution to obtain a raw material mixed solution;
2)将来自步骤1)中经过脱色处理的醋酸钠水溶液与活性炭的混合液送入醋酸钠水溶液过滤及PH调节工序经过叶片过滤机的过滤处理以后再用碱液调节PH值调整至7以后得到中性的醋酸钠水溶液,该碱液为50%的碱液,调节pH产生的废气通过吸气装置进入吸收塔吸收后排放;2) sending the mixed solution of the sodium acetate aqueous solution and activated carbon which has been decolorized in step 1) to the sodium acetate aqueous solution filtration and pH adjustment process, filtering it through a blade filter, and then adjusting the pH value to 7 with an alkali solution to obtain a neutral sodium acetate aqueous solution, wherein the alkali solution is a 50% alkali solution, and the waste gas generated by the pH adjustment enters the absorption tower through an air suction device for absorption and then is discharged;
3)将来自步骤2)中的醋酸钠水溶液送入醋酸钠水溶液蒸发工序,采用三效蒸发器蒸发,控制三效蒸发的真空度为90pa、二效蒸发的真空度为70pa、一效蒸发的真空度为40pa,控制一效蒸发温度为75℃,当蒸发好的醋酸钠浓缩液达到25°Bé时送入结晶罐结晶,控制结晶温度为55℃,结晶时间为4h,将结晶完成的料液进行离心分离,即可得到水分含量在5%的醋酸钠晶体,得到的母液再次回收利用,离心转速控制为1400rpm。3) The sodium acetate aqueous solution from step 2) is sent to the sodium acetate aqueous solution evaporation process, and a triple-effect evaporator is used for evaporation, and the vacuum degree of the triple-effect evaporation is controlled to be 90 Pa, the vacuum degree of the second-effect evaporation is controlled to be 70 Pa, and the vacuum degree of the first-effect evaporation is controlled to be 40 Pa. The temperature of the first-effect evaporation is controlled to be 75° C. When the evaporated sodium acetate concentrate reaches 25° Bé, it is sent to a crystallization tank for crystallization, and the crystallization temperature is controlled to be 55° C. The crystallization time is 4 hours. The crystallized feed liquid is centrifuged to obtain sodium acetate crystals with a moisture content of 5%. The obtained mother liquor is recycled and reused again, and the centrifugal speed is controlled to be 1400 rpm.
实施例3Example 3
本实施例提供了一种利用实施例1的系统进行醋酸钠回收处理的工艺,该工艺包括以下步骤:This embodiment provides a process for recovering sodium acetate using the system of embodiment 1, and the process comprises the following steps:
本实施例提供了一种利用实施例1的系统进行醋酸钠回收处理的工艺,该工艺包括以下步骤:This embodiment provides a process for recovering sodium acetate using the system of embodiment 1, and the process comprises the following steps:
1)将来自酸化工段的粗醋酸钠水溶液,先加入浓度为50%的液碱调节pH,将pH值调整为8,温度控制在65℃;将得到的pH值为8的粗醋酸钠水溶液送入醋酸钠水溶液脱色工序,加入活性炭进行脱色,活性炭的加入量为醋酸钠水溶液量的5%,脱色时间为1.5h,活性炭的吸附作用可将粗醋酸钠溶液中含有的油脂和胶质物及酸性物质进行脱除,得到原料混合液;1) Adding 50% liquid caustic soda to adjust the pH of the crude sodium acetate aqueous solution from the acidification section to adjust the pH value to 8, and controlling the temperature at 65° C.; sending the obtained crude sodium acetate aqueous solution with a pH value of 8 to a sodium acetate aqueous solution decolorization process, adding activated carbon for decolorization, the amount of activated carbon added is 5% of the amount of the sodium acetate aqueous solution, the decolorization time is 1.5 hours, and the adsorption effect of the activated carbon can remove the grease, colloid and acidic substances contained in the crude sodium acetate solution to obtain a raw material mixed solution;
2)将来自步骤1)中经过脱色处理的醋酸钠水溶液与活性炭的混合液送入醋酸钠水溶液过滤及PH调节工序经过叶片过滤机的过滤处理以后再调节PH值调整至7以后得到中性的醋酸钠水溶液,调节pH产生的废气通过吸气装置进入吸收塔吸收后排放;2) sending the mixed solution of the sodium acetate aqueous solution and activated carbon which has been decolorized in step 1) to the sodium acetate aqueous solution filtration and pH adjustment process, filtering it through a blade filter, and then adjusting the pH value to 7 to obtain a neutral sodium acetate aqueous solution, and the waste gas generated by the pH adjustment enters the absorption tower through an air suction device for absorption and then is discharged;
3)将来自步骤2)中的醋酸钠水溶液送入醋酸钠水溶液蒸发工序,采用三效蒸发器蒸发,控制三效蒸发的真空度为95pa、二效蒸发的真空度为75pa、一效蒸发的真空度为45pa,控制一效蒸发温度为75℃,当蒸发好的醋酸钠浓缩液达到30°Bé时送入结晶罐结晶,控制结晶温度为57℃,结晶时间为13h,将结晶完成的料液进行离心分离,即可得到水分含量在5%的醋酸钠晶体,得到的母液再次回收利用,离心转速控制为1600rpm。3) The sodium acetate aqueous solution from step 2) is sent to the sodium acetate aqueous solution evaporation process, and a triple-effect evaporator is used for evaporation, and the vacuum degree of the triple-effect evaporation is controlled to be 95 Pa, the vacuum degree of the second-effect evaporation is controlled to be 75 Pa, and the vacuum degree of the first-effect evaporation is controlled to be 45 Pa. The first-effect evaporation temperature is controlled to be 75° C. When the evaporated sodium acetate concentrate reaches 30° Bé, it is sent to a crystallization tank for crystallization, and the crystallization temperature is controlled to be 57° C. The crystallization time is 13 hours. The crystallized feed liquid is centrifuged to obtain sodium acetate crystals with a moisture content of 5%, and the obtained mother liquor is recycled and reused again, and the centrifugal speed is controlled to be 1600 rpm.
实施例4Example 4
本实施例提供了一种利用实施例1的系统进行醋酸钠回收处理的工艺,该工艺包括以下步骤:This embodiment provides a process for recovering sodium acetate using the system of embodiment 1, and the process comprises the following steps:
1)将来自酸化工段的粗醋酸钠水溶液,先加入浓度为50%的液碱调节pH,将pH值调整为9,温度控制在70℃;将得到的pH值为9的粗醋酸钠水溶液送入醋酸钠水溶液脱色工序,加入活性炭进行脱色,活性炭的加入量为醋酸钠水溶液量的10%,脱色时间为1h,活性炭的吸附作用可将粗醋酸钠溶液中含有的油脂和胶质物及酸性物质进行脱除,得到原料混合液;1) Adding 50% liquid caustic soda to adjust the pH of the crude sodium acetate aqueous solution from the acidification section to adjust the pH value to 9, and controlling the temperature at 70° C. Sending the obtained crude sodium acetate aqueous solution with a pH value of 9 to a sodium acetate aqueous solution decolorization process, adding activated carbon for decolorization, the amount of activated carbon added is 10% of the amount of the sodium acetate aqueous solution, and the decolorization time is 1 hour. The adsorption of the activated carbon can remove the grease, colloid and acidic substances contained in the crude sodium acetate solution to obtain a raw material mixed solution;
2)将来自步骤1)中经过脱色处理的醋酸钠水溶液与活性炭的混合液送入醋酸钠水溶液过滤及PH调节工序经过叶片过滤机的过滤处理以后再调节PH值调整至8以后得到碱性的醋酸钠水溶液,调节pH产生的废气通过吸气装置进入吸收塔吸收后排放;2) sending the mixed solution of the sodium acetate aqueous solution and activated carbon which has been decolorized in step 1) to the sodium acetate aqueous solution filtration and pH adjustment process, filtering it through a blade filter, and then adjusting the pH value to 8 to obtain an alkaline sodium acetate aqueous solution, and the waste gas generated by the pH adjustment enters the absorption tower through an air suction device for absorption and then is discharged;
3)将来自步骤2)中的醋酸钠水溶液送入醋酸钠水溶液蒸发工序,采用三效蒸发器蒸发,控制三效蒸发的真空度为100pa、二效蒸发的真空度为80pa、一效蒸发的真空度为50pa,控制一效蒸发温度为80℃,当蒸发好的醋酸钠浓缩液达到35°Bé时送入结晶罐结晶,控制结晶温度为60℃,结晶时间为48h,将结晶完成的料液进行离心分离,即可得到水分含量在5%的醋酸钠晶体,得到的母液再次回收利用,离心转速控制为1900rpm。3) The sodium acetate aqueous solution from step 2) is sent to the sodium acetate aqueous solution evaporation process, and a triple-effect evaporator is used for evaporation, and the vacuum degree of the triple-effect evaporation is controlled to be 100 Pa, the vacuum degree of the second-effect evaporation is controlled to be 80 Pa, and the vacuum degree of the first-effect evaporation is controlled to be 50 Pa. The temperature of the first-effect evaporation is controlled to be 80° C. When the evaporated sodium acetate concentrate reaches 35° Bé, it is sent to a crystallization tank for crystallization, and the crystallization temperature is controlled to be 60° C. The crystallization time is 48 hours. The crystallized feed liquid is centrifuged to obtain sodium acetate crystals with a moisture content of 5%. The obtained mother liquor is recycled and reused again, and the centrifugal speed is controlled to be 1900 rpm.
对比例1Comparative Example 1
本对比例与实施例4的不同之处在于:在步骤1)中,将pH值调整为11,其余步骤及工艺参数与实施例4相同。The difference between this comparative example and Example 4 is that in step 1), the pH value is adjusted to 11, and the remaining steps and process parameters are the same as those of Example 4.
对比例2Comparative Example 2
本对比例与实施例4的不同之处在于:在步骤1)中,将pH值调整为10,其余步骤及工艺参数与实施例4相同。The difference between this comparative example and Example 4 is that in step 1), the pH value is adjusted to 10, and the remaining steps and process parameters are the same as those of Example 4.
对比例3Comparative Example 3
本对比例与实施例4的不同之处在于:在步骤1)中,将pH值调整为4,其余步骤及工艺参数与实施例4相同。The difference between this comparative example and Example 4 is that in step 1), the pH value is adjusted to 4, and the remaining steps and process parameters are the same as those of Example 4.
对比例4Comparative Example 4
本对比例与实施例4的不同之处在于:在步骤1)中,将pH值调整为2,其余步骤及工艺参数与实施例4相同。The difference between this comparative example and Example 4 is that in step 1), the pH value is adjusted to 2, and the remaining steps and process parameters are the same as those of Example 4.
通过实施例2-实施例4及对比例1-4的试验实施,对所得醋酸钠的产率、醋酸钠晶体的白度、冷凝水COD进行检测,具体数据如表1所示:Through the test implementation of Example 2-Example 4 and Comparative Examples 1-4, the yield of the obtained sodium acetate, the whiteness of the sodium acetate crystals, and the COD of the condensed water were detected. The specific data are shown in Table 1:
表1Table 1
从上表可以得出,利用本回收系统和工艺方法进行油脂副产物中醋酸钠的回收,具有较高的收率,同时产品的白度基本达到市场要求,蒸发出的冷凝水的COD基本控制在300-450mg/L,同时通过对比例1-4可以看出,产品的产率相较于实施例4均降低,白度值远远低于实施例4所得到的白度,这种情况可能是由于在对比例的条件下活性炭的吸附作用低于实施例4所提出条件的吸附作用,导致醋酸钠中含有的杂质没有吸附去除彻底,从而导致对比例中产率下降及白度的降低。It can be concluded from the above table that the recovery of sodium acetate from oil by-products using the recovery system and process method has a high yield, and the whiteness of the product basically meets the market requirements, and the COD of the evaporated condensed water is basically controlled at 300-450 mg/L. At the same time, it can be seen from Comparative Examples 1-4 that the yield of the product is lower than that of Example 4, and the whiteness value is much lower than the whiteness obtained in Example 4. This may be due to the fact that the adsorption effect of the activated carbon under the conditions of the comparative example is lower than the adsorption effect under the conditions proposed in Example 4, resulting in the impurities contained in the sodium acetate not being completely adsorbed and removed, resulting in a decrease in the yield and whiteness in the comparative example.
以上所述,仅是本发明的较佳实施例而已,并非是对本发明做其他形式的限定,任何熟悉本专业的技术人员可能利用上述解释的技术内容加以变更或改型为等同变化的等效实施例用于其他领域,但是凡是未脱离本发明技术方案内容,依据本发明的技术实质对以上实施例所做的任何简单修改、等同变化与改型,仍属于本发明技术方案保护的范围。The above description is only a preferred embodiment of the present invention and does not limit the present invention in other forms. Any technician familiar with the profession may use the technical content explained above to change or modify it into an equivalent embodiment with equivalent changes for use in other fields. However, any simple modification, equivalent change and modification made to the above embodiment based on the technical essence of the present invention without departing from the content of the technical solution of the present invention still falls within the scope of protection of the technical solution of the present invention.
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