CN115650259B - Preparation method and device of large-particle sodium bicarbonate - Google Patents
Preparation method and device of large-particle sodium bicarbonate Download PDFInfo
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- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 title claims abstract description 113
- 239000002245 particle Substances 0.000 title claims abstract description 69
- 235000017557 sodium bicarbonate Nutrition 0.000 title claims abstract description 56
- 229910000030 sodium bicarbonate Inorganic materials 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 40
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 38
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 20
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 20
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract 2
- 238000005406 washing Methods 0.000 claims abstract 2
- 239000013078 crystal Substances 0.000 claims description 47
- 238000003763 carbonization Methods 0.000 claims description 32
- 238000001816 cooling Methods 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims 2
- 238000001914 filtration Methods 0.000 claims 1
- 238000005086 pumping Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 9
- 238000001631 haemodialysis Methods 0.000 abstract description 7
- 230000000322 hemodialysis Effects 0.000 abstract description 7
- 238000005119 centrifugation Methods 0.000 abstract 1
- 230000008030 elimination Effects 0.000 description 17
- 238000003379 elimination reaction Methods 0.000 description 17
- 238000000034 method Methods 0.000 description 16
- 235000017550 sodium carbonate Nutrition 0.000 description 16
- 239000000243 solution Substances 0.000 description 14
- 238000003860 storage Methods 0.000 description 14
- 238000009826 distribution Methods 0.000 description 8
- 238000002425 crystallisation Methods 0.000 description 7
- 230000008025 crystallization Effects 0.000 description 7
- 238000000502 dialysis Methods 0.000 description 7
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 6
- 238000004090 dissolution Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000006200 vaporizer Substances 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
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Abstract
本发明属于碳酸氢钠制备技术领域，具体涉及一种大颗粒碳酸氢钠的制备方法及装置。所述大颗粒碳酸氢钠的制备方法，包括以下步骤：以碳酸钠、二氧化碳为原料，制备一定浓度的碳酸钠原料液，与食品级二氧化碳反应，反应器中维持一定反应温度，物料经一定停留时间后转移至结晶器中，结晶器中保持一定温度，经一段停留时间后转移至离心机中洗涤、离心，然后干燥获得大颗粒碳酸氢钠产品。本发明制备的大颗粒碳酸氢钠产品呈梭形、近似球形，流动性较好，180‑425μm粒度范围内颗粒占比在80％以上，产品质量符合《中国药典》标准，能够满足血液透析用大颗粒碳酸氢钠的要求。The invention belongs to the technical field of sodium bicarbonate preparation, and specifically relates to a preparation method and device for large particle sodium bicarbonate. The preparation method of large particle sodium bicarbonate includes the following steps: using sodium carbonate and carbon dioxide as raw materials, preparing a sodium carbonate raw material liquid of a certain concentration, reacting with food-grade carbon dioxide, maintaining a certain reaction temperature in the reactor, and allowing the material to stay for a certain period After a certain period of time, it is transferred to the crystallizer. The crystallizer is kept at a certain temperature. After a period of residence, it is transferred to a centrifuge for washing, centrifugation, and then drying to obtain a large particle sodium bicarbonate product. The large-particle sodium bicarbonate product prepared by the invention is fusiform, approximately spherical, has good fluidity, and the proportion of particles in the 180-425 μm particle size range is more than 80%. The product quality meets the standards of the "Chinese Pharmacopoeia" and can meet the needs of hemodialysis. Requirements for large particle size sodium bicarbonate.
Description
技术领域Technical field
本发明属于碳酸氢钠制备技术领域，具体涉及一种大颗粒碳酸氢钠的制备方法及装置。The invention belongs to the technical field of sodium bicarbonate preparation, and specifically relates to a preparation method and device for large particle sodium bicarbonate.
背景技术Background technique
碳酸氢钠，即小苏打是一种重要的无机化工产品，广泛应用于各个产业中，在国民经济中占有重要地位。对于传统碳酸氢钠的生产，国内已形成相当的工业规模，但近年来，我国关于碳酸氢钠产品消费结构逐渐发生变化，对高端小苏打产品需求上升较快，导致国内高端小苏打产品生产短缺问题日渐突出。Sodium bicarbonate, also known as baking soda, is an important inorganic chemical product that is widely used in various industries and occupies an important position in the national economy. For the production of traditional sodium bicarbonate, a considerable industrial scale has been formed in China. However, in recent years, my country's consumption structure of sodium bicarbonate products has gradually changed, and the demand for high-end baking soda products has increased rapidly, resulting in a shortage of domestic high-end baking soda products. The problem is becoming increasingly prominent.
透析、注射用碳酸氢钠是小苏打系列产品中重要的品种之一，其主要应用于血液透析场景中。透析液作为血液透析系统的重要组成部分，其主要作用是纠正患者内环境电解质紊乱、维持酸碱平衡。血液透析浓缩液可分为酸性透析浓缩液(A液)和碱性透析浓缩液(B液)，A液为氯化钠、氯化钾、氯化钙、氯化镁、冰醋酸溶液，B液为碳酸氢钠溶液。在具体使用场景中，B液可分为两种方式制备，一种是现配现用，将浓缩碳酸氢钠干粉溶解后使用，另一种是将颗粒碳酸氢钠装填进柱或者袋中，在透析机上实现B液的连续配制。碳酸氢钠溶液在贮存和运输过程中可能会产生一定程度分解，液体贮存和运输不便且存在生物危险的风险，由于以上原因，采用颗粒碳酸氢钠在上机时实现B液的连续配制越来越受到市场的推崇。但此方法对碳酸氢钠颗粒要求较高，粉末状碳酸氢钠颗粒小、溶解时易结块、流动性差，不仅不利于碳酸氢钠的快速溶解，还极易在透析过程中堵塞导管，目前国内药用碳酸氢钠厂家生产的产品粒度均较小，达不到上机标准，国内血液透析用大颗粒碳酸氢钠均为进口产品，因此填补国内市场透析用大颗粒碳酸氢钠产品空白已经迫在眉睫。Sodium bicarbonate for dialysis and injection is one of the important varieties in the baking soda series products, and it is mainly used in hemodialysis scenarios. As an important part of the hemodialysis system, dialysate's main function is to correct electrolyte disorders in the patient's internal environment and maintain acid-base balance. Hemodialysis concentrate can be divided into acidic dialysis concentrate (Liquid A) and alkaline dialysis concentrate (Liquid B). Liquid A is sodium chloride, potassium chloride, calcium chloride, magnesium chloride, and glacial acetic acid solution. Liquid B is Sodium bicarbonate solution. In specific usage scenarios, Liquid B can be prepared in two ways. One is to prepare it immediately and use it after dissolving the concentrated dry powder of sodium bicarbonate. The other is to pack granular sodium bicarbonate into a column or bag. Realize the continuous preparation of B solution on the dialysis machine. Sodium bicarbonate solution may decompose to a certain extent during storage and transportation, which makes liquid storage and transportation inconvenient and poses a risk of biohazard. Due to the above reasons, it is more and more popular to use granular sodium bicarbonate to achieve continuous preparation of liquid B when putting it on the machine. The more it is respected by the market. However, this method has higher requirements for sodium bicarbonate particles. Powdered sodium bicarbonate particles are small, easy to agglomerate when dissolved, and have poor fluidity. This is not only not conducive to the rapid dissolution of sodium bicarbonate, but also easily blocks the catheter during dialysis. At present, The particle size of the products produced by domestic medicinal sodium bicarbonate manufacturers is small and cannot meet the machine-ready standards. Domestic large-particle sodium bicarbonate for hemodialysis is an imported product. Therefore, the gap in large-particle sodium bicarbonate for dialysis in the domestic market has been filled. Imminent.
专利CN206428008U利用重结晶方法，在90℃条件下配制一定组成原料液，随后在30～40℃条件下进行结晶，大颗粒产品粒度范围在180-425μm内，但关于产品形貌及粒度分布均未提及。The patent CN206428008U uses the recrystallization method to prepare a certain composition of raw material liquid at 90°C, and then crystallizes at 30 to 40°C. The particle size range of the large particle product is 180-425 μm, but the product morphology and particle size distribution are unknown. mentioned.
专利CN206428007U以纯碱以及食品级二氧化碳为原料，通过在结晶器中进行反应，反应及结晶过程恒定温度为25℃，并每隔40分钟排出体系中细晶，反应时间6小时，滞留反应液24小时后取出产品。所得产品180-425μm范围内产品占比能够达到60％，但用于血液透析的大颗粒碳酸氢钠产品需具有规则的形貌，对颗粒堆积性能有一定要求，但该专利中未给出产品形貌。Patent CN206428007U uses soda ash and food-grade carbon dioxide as raw materials, and reacts in a crystallizer. The constant temperature of the reaction and crystallization process is 25°C, and the fine crystals in the system are discharged every 40 minutes. The reaction time is 6 hours, and the reaction liquid is retained for 24 hours. Then remove the product. The proportion of products in the 180-425μm range of the obtained product can reach 60%, but the large-particle sodium bicarbonate product used for hemodialysis needs to have a regular morphology and has certain requirements for particle accumulation performance, but the product is not given in the patent Appearance.
专利CN105819471B公开了一种生产大粒度小苏打的方法，以纯碱碳化法作为基础，对工艺中关键设备反应结晶器进行创新设计，并结合细晶消除、添加晶种的方式获得了粒度分布满意的产品，其中粒径大于180μm占比75％以上，但颗粒形貌呈现长棒状，区别于近似球形、梭形颗粒产品，可能会产生堆密度较小，上机效果较差的问题。Patent CN105819471B discloses a method for producing large-grained baking soda. Based on the soda ash carbonization method, an innovative design of the reaction crystallizer, a key equipment in the process, is combined with the elimination of fine crystals and the addition of seed crystals to obtain satisfactory particle size distribution. Products with particle sizes greater than 180 μm account for more than 75%, but the particle morphology is long rod-shaped, which is different from approximately spherical and fusiform particle products, which may cause problems such as smaller bulk density and poor machine performance.
发明内容Contents of the invention
本发明解决的技术问题是：提供了一种大颗粒碳酸氢钠的制备方法，产品呈梭形、近似球形，流动性较好，粒度在180-425μm的颗粒占比在80％以上，满足《中国药典》中关于药用碳酸氢钠相关标准，同时满足血液透析用碳酸氢钠的临床要求；本发明还提供其制备方法。The technical problem solved by the present invention is to provide a method for preparing large particles of sodium bicarbonate. The product is fusiform, approximately spherical, has good fluidity, and the particles with a particle size of 180-425 μm account for more than 80%, meeting the requirements of " The relevant standards for medicinal sodium bicarbonate in the Chinese Pharmacopoeia also meet the clinical requirements of sodium bicarbonate for hemodialysis; the invention also provides a preparation method thereof.
本发明所述的大颗粒碳酸氢钠的制备方法，包括以下步骤：The preparation method of large particle sodium bicarbonate according to the present invention includes the following steps:
配制一定浓度的碳酸钠溶液过滤后泵入碳化反应器中，并通入二氧化碳，在70-90℃下进行气液两相反应，物料经一定停留时间后转移至结晶器中，在20-70℃温度下进行降温结晶，同时可采用细晶消除罐对结晶器中的细晶采出、溶解后返回结晶器，物料经一定停留时间后转移至离心机中，洗涤、离心，干燥获得大颗粒碳酸氢钠产品。Prepare a sodium carbonate solution of a certain concentration, filter it, and pump it into the carbonization reactor, and introduce carbon dioxide to carry out a gas-liquid two-phase reaction at 70-90°C. After a certain residence time, the material is transferred to the crystallizer, and is heated at 20-70 Cooling crystallization is carried out at ℃ temperature. At the same time, a fine crystal elimination tank can be used to extract the fine crystals in the crystallizer, dissolve them and return them to the crystallizer. After a certain residence time, the materials are transferred to a centrifuge, washed, centrifuged, and dried to obtain large particles. Sodium bicarbonate products.
本发明中，所述碳酸钠溶液浓度为10-20wt％。In the present invention, the concentration of the sodium carbonate solution is 10-20wt%.
本发明中，所述二氧化碳优选食品级二氧化碳。In the present invention, the carbon dioxide is preferably food grade carbon dioxide.
本发明中，所述碳化反应器内物料停留时间为0.2-3h。In the present invention, the residence time of materials in the carbonization reactor is 0.2-3h.
碳化过程中存在一定的晶体析出，此部分晶体可作为结晶器内的晶种。There is a certain amount of crystal precipitation during the carbonization process, and this part of the crystal can be used as seed crystal in the crystallizer.
本发明中，所述结晶器内物料停留时间为2-8h。In the present invention, the residence time of materials in the crystallizer is 2-8 hours.
本发明中，所述细晶消除罐内的温度为75-85℃。In the present invention, the temperature in the fine crystal elimination tank is 75-85°C.
在结晶器中，晶体成核、生长的同时，采用细晶消除方式，将小于180μm的细晶进行采出，在细晶消除罐内以较高温度快速溶解后，再返回结晶器进行结晶，从而对体系内晶体进行粒度重整优化。In the crystallizer, while the crystals are nucleating and growing, fine crystals smaller than 180 μm are extracted using the fine grain elimination method. After being rapidly dissolved at a higher temperature in the fine grain elimination tank, they are then returned to the crystallizer for crystallization. Thus, the particle size reforming of the crystals in the system is optimized.
本发明中，制备得到的大颗粒碳酸氢钠晶体形貌为梭形或类球体，粒度在180-425μm的颗粒占比在80％以上，流动性较好，具有一定颗粒强度。In the present invention, the morphology of the prepared large-particle sodium bicarbonate crystals is spindle-shaped or spherical-like, and the proportion of particles with a particle size of 180-425 μm is more than 80%. It has good fluidity and a certain particle strength.
本发明所述的大颗粒碳酸氢钠的制备方法所用的装置，包括食品级二氧化碳储罐、碳酸钠溶液储罐、碳化反应器、结晶器以及细晶消除罐，所述碳化反应器的进料口连接食品级二氧化碳储罐和碳酸钠溶液储罐，所述碳化反应器的出料口连接结晶器的进料口，所述结晶器的顶部与细晶消除罐循环相连，结晶器的底部出料口依次连接离心机和气流干燥机。The device used in the preparation method of large particle sodium bicarbonate of the present invention includes a food-grade carbon dioxide storage tank, a sodium carbonate solution storage tank, a carbonization reactor, a crystallizer and a fine crystal elimination tank. The feed of the carbonization reactor The port is connected to the food-grade carbon dioxide storage tank and the sodium carbonate solution storage tank. The outlet of the carbonization reactor is connected to the feed port of the crystallizer. The top of the crystallizer is cyclically connected to the fine crystal elimination tank, and the bottom outlet of the crystallizer The material port is connected to the centrifuge and the airflow dryer in turn.
所述结晶器和细晶消除罐均带有夹套，通过公用工程进行控温。The crystallizer and the fine crystal elimination tank are both equipped with jackets, and the temperature is controlled through public works.
所述食品级二氧化碳储罐和碳化反应器之间设置有二氧化碳汽化器。A carbon dioxide vaporizer is provided between the food-grade carbon dioxide storage tank and the carbonization reactor.
其中，所述碳化反应器内反应温度通过进料温度进行控制，细晶消除罐、结晶器通过公用工程维持在恒温状态。Among them, the reaction temperature in the carbonization reactor is controlled by the feed temperature, and the fine crystal elimination tank and crystallizer are maintained at a constant temperature through public works.
与现有技术相比，本发明的有益效果如下：Compared with the prior art, the beneficial effects of the present invention are as follows:
(1)本发明基于纯碱碳化法制备颗粒碳酸氢钠，采用将碳化过程与结晶过程分离的基本思路，通过碳化反应得到形貌、分布较为适宜的基本粒子，进一步转移至结晶器中生长，从而制备颗粒碳酸氢钠；(1) The present invention prepares granular sodium bicarbonate based on the soda ash carbonization method. It adopts the basic idea of separating the carbonization process and the crystallization process. Basic particles with suitable morphology and distribution are obtained through the carbonization reaction, and are further transferred to the crystallizer for growth, thereby Preparation of granular sodium bicarbonate;
(2)本发明制备的大颗粒碳酸氢钠形貌、粒度分布及晶体强度满足透析用颗粒碳酸氢钠产品的要求，在过程中无需加入任何添加剂，产品质量符合国家药典中对于医药级碳酸氢钠的基本要求；(2) The morphology, particle size distribution and crystal strength of the large-granule sodium bicarbonate prepared by the present invention meet the requirements of granular sodium bicarbonate products for dialysis. No additives need to be added during the process. The product quality meets the requirements for pharmaceutical grade bicarbonate in the National Pharmacopoeia. Basic Sodium Requirements;
(3)本发明所述工艺步骤简单，制备大颗粒碳酸氢钠有效、可靠，具有一定生产效率，可以进一步放大生产。(3) The process steps described in the present invention are simple, the preparation of large particles of sodium bicarbonate is effective and reliable, has a certain production efficiency, and can further scale up production.
附图说明Description of drawings
图1为本发明实施例1制备的碳酸氢钠晶体的SEM图；Figure 1 is an SEM image of sodium bicarbonate crystal prepared in Example 1 of the present invention;
图2为本发明实施例2制备的碳酸氢钠晶体的SEM图；Figure 2 is an SEM image of sodium bicarbonate crystals prepared in Example 2 of the present invention;
图3为本发明实施例1制备的碳酸氢钠晶体粒度分布图；Figure 3 is a particle size distribution diagram of sodium bicarbonate crystals prepared in Example 1 of the present invention;
图4为本发明实施例2制备的碳酸氢钠晶体粒度分布图；Figure 4 is a particle size distribution diagram of sodium bicarbonate crystals prepared in Example 2 of the present invention;
图5为市售碳酸氢钠晶体的SEM图；Figure 5 is an SEM image of commercially available sodium bicarbonate crystals;
图6为本发明大颗粒碳酸氢钠的制备装置结构示意图；Figure 6 is a schematic structural diagram of a device for preparing large particle sodium bicarbonate of the present invention;
图中：1、食品级二氧化碳储罐；2、碳酸钠溶液储罐；3、碳化反应器；4、结晶器；5、细晶消除罐；6离心机；7、气流干燥机；8、二氧化碳汽化器。In the picture: 1. Food grade carbon dioxide storage tank; 2. Sodium carbonate solution storage tank; 3. Carbonization reactor; 4. Crystallizer; 5. Fine crystal elimination tank; 6. Centrifuge; 7. Air flow dryer; 8. Carbon dioxide Carburetor.
具体实施方式Detailed ways
下面结合实施例对本发明作进一步说明，实施例中所使用的原料，如无特别说明，均为市售常规原料；实施例中所使用的工艺方法，如无特别说明，均为本领域常规方法。The present invention will be further described below with reference to the examples. The raw materials used in the examples, unless otherwise stated, are all commercially available conventional raw materials. The process methods used in the examples, unless otherwise stated, are all conventional methods in this field. .
实施例1Example 1
如图6所示，一种大颗粒碳酸氢钠的制备装置，包括食品级二氧化碳储罐1、碳酸钠溶液储罐2、碳化反应器3、结晶器4以及细晶消除罐5，所述碳化反应器3的进料口连接食品级二氧化碳储罐1和碳酸钠溶液储罐2，所述碳化反应器3的出料口连接结晶器4的进料口，所述结晶器4的顶部与细晶消除罐5循环相连，结晶器4的底部出料口依次连接离心机6和气流干燥机7。As shown in Figure 6, a device for preparing large particle sodium bicarbonate includes a food-grade carbon dioxide storage tank 1, a sodium carbonate solution storage tank 2, a carbonization reactor 3, a crystallizer 4 and a fine crystal elimination tank 5. The carbonization The feed port of the reactor 3 is connected to the food-grade carbon dioxide storage tank 1 and the sodium carbonate solution storage tank 2. The discharge port of the carbonization reactor 3 is connected to the feed port of the crystallizer 4. The top of the crystallizer 4 is connected to the fine The crystal elimination tank 5 is connected cyclically, and the bottom outlet of the crystallizer 4 is connected to the centrifuge 6 and the air flow dryer 7 in sequence.
所述结晶器4和细晶消除罐5均带有夹套，通过公用工程进行控温。The crystallizer 4 and the fine crystal elimination tank 5 are both equipped with jackets, and the temperature is controlled through public works.
所述食品级二氧化碳储罐1和碳化反应器3之间设置有二氧化碳汽化器8。A carbon dioxide vaporizer 8 is provided between the food-grade carbon dioxide storage tank 1 and the carbonization reactor 3 .
其中，所述碳化反应器3内反应温度通过进料温度进行控制，细晶消除罐5、结晶器4通过公用工程维持在恒温状态。Among them, the reaction temperature in the carbonization reactor 3 is controlled by the feed temperature, and the fine crystal elimination tank 5 and the crystallizer 4 are maintained at a constant temperature through public works.
实施例2Example 2
采用实施例1中所述的装置制备大颗粒碳酸氢钠，步骤如下：The device described in Example 1 is used to prepare large particle sodium bicarbonate, and the steps are as follows:
以碳酸钠为原料，配制浓度为12wt％的碳酸钠溶液过滤，以0.6m3/h的速率通入碳化反应器中，同时将食品级二氧化碳以60.8Nm3/h的速率通入碳化反应器中，保持碳化反应器内反应温度为70℃，物料在碳化反应器内停留1.5h后转移至结晶器中，结晶器内温度保持在20℃，进行结晶，同时采用细晶消除罐对结晶器中粒径小于180μm的析晶采出、溶解(溶解温度75℃)后返回结晶器，物料在结晶器内停留4h后，转移至离心机中，进行洗涤、离心，然后干燥获得大颗粒碳酸氢钠产品。Using sodium carbonate as raw material, prepare a sodium carbonate solution with a concentration of 12wt%, filter it, and pass it into the carbonization reactor at a rate of 0.6m 3 /h. At the same time, feed food-grade carbon dioxide into the carbonization reactor at a rate of 60.8Nm 3 /h. , the reaction temperature in the carbonization reactor is kept at 70°C. The material stays in the carbonization reactor for 1.5 hours and then transferred to the crystallizer. The temperature in the crystallizer is maintained at 20°C for crystallization. At the same time, a fine crystal elimination tank is used to clean the crystallizer. The crystals with a medium particle size less than 180 μm are extracted, dissolved (dissolution temperature 75°C) and returned to the crystallizer. After the material stays in the crystallizer for 4 hours, it is transferred to a centrifuge, washed, centrifuged, and then dried to obtain large particles of hydrogen carbonate. Sodium Products.
制备的大颗粒碳酸氢钠晶体微观形态如图1所示，晶体粒度分布如图3所示，可以看到，制备的大颗粒碳酸氢钠晶体形貌为梭形或类球体，粒度在180-425μm的颗粒占比为87.9％。The microscopic morphology of the prepared large-particle sodium bicarbonate crystals is shown in Figure 1, and the crystal particle size distribution is shown in Figure 3. It can be seen that the prepared large-particle sodium bicarbonate crystals are fusiform or quasi-spherical in shape, with a particle size of 180- The proportion of 425 μm particles is 87.9%.
实施例3Example 3
采用实施例1中所述的装置制备大颗粒碳酸氢钠，步骤如下：The device described in Example 1 is used to prepare large particle sodium bicarbonate, and the steps are as follows:
以碳酸钠为原料，配制浓度为15wt％的碳酸钠溶液过滤，以0.6m3/h的速率通入碳化反应器中，同时将食品级二氧化碳以57.0Nm3/h的速率通入碳化反应器中，保持碳化反应器内反应温度为80℃，物料在碳化反应器内停留0.2h后转移至结晶器中，结晶器内温度保持在50℃，进行结晶，同时采用细晶消除罐对结晶器中粒径小于180μm的析晶采出、溶解(溶解温度60℃)后返回结晶器，物料在结晶器内停留2h后，转移至离心机中，进行洗涤、离心，然后干燥获得大颗粒碳酸氢钠产品。Using sodium carbonate as raw material, prepare a sodium carbonate solution with a concentration of 15wt%, filter it, and pass it into the carbonization reactor at a rate of 0.6m 3 /h. At the same time, feed food-grade carbon dioxide into the carbonization reactor at a rate of 57.0Nm 3 /h. , keep the reaction temperature in the carbonization reactor at 80°C, and transfer the material to the crystallizer after staying in the carbonization reactor for 0.2h. The temperature in the crystallizer is maintained at 50°C for crystallization. At the same time, a fine crystal elimination tank is used to clean the crystallizer. The crystals with a medium particle size less than 180 μm are extracted, dissolved (dissolution temperature 60°C) and returned to the crystallizer. After the material stays in the crystallizer for 2 hours, it is transferred to a centrifuge, washed, centrifuged, and then dried to obtain large particles of hydrogen carbonate. Sodium Products.
制备的大颗粒碳酸氢钠晶体微观形态如图2所示，晶体粒度分布如图4所示，可以看到，制备的大颗粒碳酸氢钠晶体形貌为梭形或类球体，粒度在180-425μm的颗粒占比为88.1％。The microscopic morphology of the prepared large-particle sodium bicarbonate crystals is shown in Figure 2, and the crystal particle size distribution is shown in Figure 4. It can be seen that the prepared large-particle sodium bicarbonate crystals are fusiform or spherical in shape, with a particle size of 180- The proportion of 425 μm particles is 88.1%.
实施例4Example 4
采用实施例1中所述的装置制备大颗粒碳酸氢钠，步骤如下：The device described in Example 1 is used to prepare large particle sodium bicarbonate, and the steps are as follows:
以碳酸钠为原料，配制浓度为20wt％的碳酸钠溶液过滤，以0.6m3/h的速率通入碳化反应器中，同时将食品级二氧化碳以50.6Nm3/h的速率通入碳化反应器中，保持碳化反应器内反应温度为90℃，物料在碳化反应器内停留3h后转移至结晶器中，结晶器内温度保持在70℃，进行结晶，同时采用细晶消除罐对结晶器中粒径小于180μm的析晶采出、溶解(溶解温度80℃)后返回结晶器，物料在结晶器内停留8h后，转移至离心机中，进行洗涤、离心，然后干燥获得大颗粒碳酸氢钠产品。Using sodium carbonate as raw material, prepare a sodium carbonate solution with a concentration of 20wt%, filter it, and pass it into the carbonization reactor at a rate of 0.6m 3 /h. At the same time, feed food-grade carbon dioxide into the carbonization reactor at a rate of 50.6Nm 3 /h. , keep the reaction temperature in the carbonization reactor at 90°C, and transfer the material to the crystallizer after staying in the carbonization reactor for 3 hours. The temperature in the crystallizer is maintained at 70°C for crystallization. At the same time, a fine crystal elimination tank is used to clean the crystallizer. The crystals with a particle size less than 180 μm are extracted, dissolved (dissolution temperature 80°C) and returned to the crystallizer. After the material stays in the crystallizer for 8 hours, it is transferred to a centrifuge, washed, centrifuged, and then dried to obtain large particles of sodium bicarbonate. product.
制备的大颗粒碳酸氢钠晶体形貌为梭形或类球体，粒度在180-425μm的颗粒占比为87.2％。The morphology of the prepared large-particle sodium bicarbonate crystals is fusiform or spherical, and the proportion of particles with a particle size of 180-425 μm is 87.2%.
对比例1Comparative example 1
市售碳酸氢钠。Commercially available sodium bicarbonate.
市售碳酸氢钠晶体的微观形态如图5所示，可以看出，其晶体形貌不规则，颗粒大小均匀性差，且细颗粒含量较高。The microscopic morphology of commercially available sodium bicarbonate crystals is shown in Figure 5. It can be seen that the crystal morphology is irregular, the particle size uniformity is poor, and the content of fine particles is high.
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