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申请号:201911293144.X 公开号:CN110980833A 主分类号:C02F1/00
摘要:【中文】本发明公开了一种电子级氯化亚铁的制备方法。其目的是为了提供一种生产原理简单、原料来源广泛、成本低廉且易于进行工业化生产的电子级氯化亚铁的生产方法。本发明将经过预处理且已还原除杂的含铁废盐酸打进三效蒸发系统进行蒸发浓缩,再经过冷却降温、离心过滤得到四水氯化亚铁结晶,如果结晶未达到电子级氯化亚铁的控制指标,再用多次重结晶方法直至得到达到控制标准的电子级氯化亚铁,而且离心后的母液可直接用于生产水处理剂三氯化铁,整个过程不产生二次污染物。同时避免了传统生产工艺中亚铁离子在较高温度下极易氧化成三价铁以及酸度不足时易造成三价铁水解,产品变黄,不易储存等不足。本发明用于能源材料制备技术领域。 【EN】The invention discloses a preparation method of electronic grade ferrous chloride. The method for producing the electronic grade ferrous chloride has the advantages of simple production principle, wide raw material source, low cost and easy industrial production. The method comprises the steps of pumping the iron-containing waste hydrochloric acid which is subjected to pretreatment and reduction impurity removal into a three-effect evaporation system for evaporation concentration, cooling, centrifuging and filtering to obtain ferrous chloride tetrahydrate crystals, and if the crystals do not reach the control index of the electronic-grade ferrous chloride, performing repeated recrystallization until the electronic-grade ferrous chloride reaching the control standard is obtained, wherein the centrifuged mother liquor can be directly used for producing the water treatment agent ferric chloride, and no secondary pollutant is generated in the whole process. Meanwhile, the defects that ferrous ions are easily oxidized into ferric iron at a higher temperature and ferric iron is easily hydrolyzed when the acidity is insufficient, the product turns yellow, and the storage is difficult in the traditional production process are avoided. The invention is used in the technical field of energy material preparation.
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申请号:201911375410.3 公开号:CN111018001A 主分类号:C01G49/10
摘要:【中文】本发明公开了一种处理热镀锌废盐酸的工艺方法,包括将经过预处理且已还原除杂的热镀锌废盐酸打进三效蒸发系统进行蒸发浓缩,再经过冷却降温、离心过滤得到固体氯化亚铁和母液。如果固体氯化亚铁中的锌含量不超过控制指标,用于生产符合国标要求的水处理剂三氯化铁产品,反之,需要用蒸发浓缩产生的稀酸水溶解后再经过重结晶以得到锌含量符合控制指标的固体氯化亚铁,进而生产符合国标要求的水处理剂三氯化铁产品。本发明的技术方案工艺简单,操作危险系数低,不会产生二次污染,为热镀锌废盐酸的资源化利用提供了新的途径,有效地降低了环保压力,同时增加了企业的经济效益。 【EN】The invention discloses a process method for treating hot galvanizing waste hydrochloric acid, which comprises the steps of pumping the hot galvanizing waste hydrochloric acid which is pretreated and reduced to remove impurities into a triple-effect evaporation system for evaporation and concentration, and then cooling and centrifugally filtering to obtain solid ferrous chloride and mother liquor. If the zinc content in the solid ferrous chloride does not exceed the control index, the solid ferrous chloride is used for producing the water treatment agent ferric trichloride product meeting the national standard requirement, otherwise, the solid ferrous chloride with the zinc content meeting the control index is obtained by being dissolved by dilute acid water generated by evaporation and concentration and then being recrystallized, and the water treatment agent ferric trichloride product meeting the national standard requirement is further produced. The technical scheme of the invention has simple process and low operation risk coefficient, does not generate secondary pollution, provides a new way for the resource utilization of the hot galvanizing waste hydrochloric acid, effectively reduces the environmental protection pressure and increases the economic benefit of enterprises at the same time.
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申请号:202010012854.7 公开号:CN111018002A 主分类号:C01G49/10
摘要:【中文】本发明涉及一种大颗粒六水氯化铁的制备方法,其包括以下步骤:将固体氯化亚铁在温度60~80℃溶解制得饱和氯化亚铁溶液,采用氯气氧化可得铁离子质量分数为17.50%~18.25%的氯化铁溶液。对氯化铁溶液进行快速搅拌、冷水降温至24~25℃,再依次进行投加晶种、慢速搅拌、逐步降温操作,使氯化铁溶液在低饱和度下逐渐析出结晶,再进行离心分离可获得大颗粒六水氯化铁结晶。本发明方法克服了传统六水氯化铁工艺中产品纯度低、过程复杂、母液易结晶堵管、离心回收率低的问题。本发明具有工艺简单、操作方便、成本费用低的特点,便于六水氯化铁工业化生产控制,提高了生产效率。 【EN】The invention relates to a preparation method of large-particle ferric chloride hexahydrate, which comprises the following steps: dissolving solid ferrous chloride at the temperature of 60-80 ℃ to prepare a saturated ferrous chloride solution, and oxidizing by adopting chlorine gas to obtain the ferric chloride solution with the ferric ion mass fraction of 17.50% -18.25%. Rapidly stirring the ferric chloride solution, cooling the ferric chloride solution to 24-25 ℃ with cold water, then sequentially adding seed crystals, slowly stirring and gradually cooling to gradually separate out crystals from the ferric chloride solution at a low saturation degree, and then carrying out centrifugal separation to obtain large-particle ferric chloride hexahydrate crystals. The method provided by the invention overcomes the problems of low product purity, complex process, easy crystallization of mother liquor, pipe blockage and low centrifugal recovery rate in the traditional ferric chloride hexahydrate process. The method has the characteristics of simple process, convenient operation and low cost, is convenient for industrial production control of the ferric chloride hexahydrate, and improves the production efficiency.
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申请号:202010012835.4 公开号:CN111170373A 主分类号:C01G49/10
摘要:【中文】本发明涉及一种四水氯化亚铁的制备方法,其包括以下步骤:采用盐酸酸洗废液溶解钢铁氧化皮,再与还原铁粉进行置换反应,过滤得到氯化亚铁溶液;将所述的氯化亚铁溶液依次进行蒸发浓缩、降温结晶、离心分离,获得四水氯化亚铁。本发明的方法克服传统四水氯化亚铁工艺中产品纯度低、颗粒小、离心回收率低的问题。本发明方法具有工艺简单、操作方便、成本费用低的特点,不仅实现盐酸洗废液资源化和无害化处理,而且有良好的经济和环境效益。 【EN】The invention relates to a preparation method of ferrous chloride tetrahydrate, which comprises the following steps: dissolving iron and steel oxide skin by using hydrochloric acid pickling waste liquor, performing replacement reaction on the iron and steel oxide skin and reduced iron powder, and filtering to obtain a ferrous chloride solution; and sequentially carrying out evaporation concentration, cooling crystallization and centrifugal separation on the ferrous chloride solution to obtain ferrous chloride tetrahydrate. The method of the invention overcomes the problems of low product purity, small particles and low centrifugal recovery rate in the traditional ferrous chloride tetrahydrate process. The method has the characteristics of simple process, convenient operation and low cost, realizes the recycling and harmless treatment of the pickling waste liquor, and has good economic and environmental benefits.
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申请号:202010012846.2 公开号:CN111170430A 主分类号:C02F1/52
摘要:【中文】本发明涉及一种块状聚氯化铁固体的生产方法,其包括以下步骤:向反应釜中加入盐酸溶液与氯化亚铁固体,开启搅拌,加入稳定剂,通过氧化反应获得聚氯化铁溶液;对聚氯化铁溶液进行快速搅拌冷却至物料温25~27℃,随后加入晶种,继续搅拌30~90min,得到含晶粒的聚氯化铁溶液;将其转置于多边形塑料模具中,在低温环境下静置4~6小时,可获得块状聚氯化铁固体。本发明方法工艺简单,操作方便;所得的产品杂质含量低、铁含量较高,水溶解性清澈透亮,实用价值较高;固体易于运输和保存,具有良好的应用前景。 【EN】The invention relates to a method for producing blocky polyferric chloride solid, which comprises the following steps: adding a hydrochloric acid solution and ferrous chloride solid into a reaction kettle, starting stirring, adding a stabilizer, and obtaining a poly ferric chloride solution through an oxidation reaction; rapidly stirring and cooling the poly-ferric chloride solution to a material temperature of 25-27 ℃, then adding seed crystals, and continuously stirring for 30-90 min to obtain a poly-ferric chloride solution containing crystal grains; and (3) transferring the solid product into a polygonal plastic mould, and standing for 4-6 hours in a low-temperature environment to obtain a blocky polyferric chloride solid. The method has simple process and convenient operation; the obtained product has low impurity content, high iron content, clear and transparent water solubility and high practical value; the solid is easy to transport and store, and has good application prospect.
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申请号:202010012874.4 公开号:CN111153477A 主分类号:C02F1/52
摘要:【中文】本发明涉及一种粉状聚氯化铁固体的制备方法,其包括以下步骤:向盐酸酸洗废液中加入钢铁氧化皮,搅拌加热至50~60℃,反应1.5~3.0小时,经过滤、氧化、蒸发后,制得聚氯化铁浓缩液;对聚氯化铁浓缩液进行搅拌冷却,加入晶种,慢速搅拌降温22~20℃,得到含晶粒聚氯化铁溶液;对所述含晶粒的聚氯化铁进行固液分离,获得粉状聚氯化铁固体。本发明方法利用盐酸酸洗废液与钢铁氧化皮制备粉状聚氯化铁固体,变废为宝,实现资源的充分利用。本发明方法具有工艺简单,成本低,所得固体产品铁含量较高,水溶性好,能更加有效应用于废水处理中。 【EN】The invention relates to a preparation method of powdery polyferric chloride solid, which comprises the following steps: adding iron oxide skin into the hydrochloric acid pickling waste liquid, stirring and heating to 50-60 ℃, reacting for 1.5-3.0 hours, and filtering, oxidizing and evaporating to obtain a poly-ferric chloride concentrated solution; stirring and cooling the concentrated solution of the poly-ferric chloride, adding seed crystals, slowly stirring and cooling for 22-20 ℃ to obtain a poly-ferric chloride solution containing crystal grains; and carrying out solid-liquid separation on the poly-ferric chloride containing the crystal grains to obtain powdery poly-ferric chloride solid. The method utilizes the hydrochloric acid pickling waste liquid and the steel oxide skin to prepare the powdery polyferric chloride solid, changes waste into valuable, and realizes the full utilization of resources. The method has the advantages of simple process, low cost, high iron content of the obtained solid product, good water solubility and more effective application in wastewater treatment.
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申请号:201911300034.1 公开号:CN111056573A 主分类号:C01G49/10
摘要:【中文】本发明公开一种结晶氯化铁连续生产工艺。该生产工艺包括如下步骤:将低浓度氯化铁在蒸发系统浓缩到55~65%;浓缩液经过冷却器冷却到35~45℃持续转入第一级结晶釜冷却,在第一级结晶釜的浓缩液冷却到25~35℃时,向第一级结晶釜中按每立方米浓缩液中加入5~10kg结晶氯化铁的比例添加晶种;加入晶种后的物料自第一级结晶釜增长到3~10%持续转入第二级结晶釜后继续冷却结晶;将在第二级结晶釜晶体增长到10~25%的浓缩液持续转入第三级结晶釜,浓缩液在第三级结晶釜继续冷却达到25~50%结晶的设计比例;达到设计结晶比例的浓缩液持续转入自动离心机进行连续离心分离得到颗粒状结晶氯化铁产品。 【EN】The invention discloses a continuous production process of crystalline ferric chloride. The production process comprises the following steps: concentrating the low-concentration ferric chloride to 55-65% in an evaporation system; cooling the concentrated solution to 35-45 ℃ through a cooler, continuously transferring the concentrated solution into a first-stage crystallization kettle for cooling, and adding seed crystals into the first-stage crystallization kettle according to the proportion of adding 5-10 kg of crystalline ferric chloride into each cubic meter of the concentrated solution when the concentrated solution in the first-stage crystallization kettle is cooled to 25-35 ℃; the material added with the seed crystals is increased to 3-10% from the first-stage crystallization kettle and continuously transferred to the second-stage crystallization kettle, and then cooling and crystallization are continuously carried out; continuously transferring the concentrated solution with the crystal growing to 10-25% in the second-stage crystallization kettle into a third-stage crystallization kettle, and continuously cooling the concentrated solution in the third-stage crystallization kettle to reach the design proportion of 25-50% crystallization; and continuously transferring the concentrated solution reaching the designed crystallization ratio into an automatic centrifuge for continuous centrifugal separation to obtain granular crystallized ferric chloride products.
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申请号:201911377989.7 公开号:CN110950389A 主分类号:C01G49/10
摘要:【中文】本发明公开一种颗粒状二水合氯化亚铁的生产工艺,包括如下步骤:将压滤后的氯化亚铁溶液连续经过蒸发浓缩后得到的氯化亚铁浓缩液以2~8t/h的出料速度连续进入一个夹套带冷却水的结晶釜进行冷却;氯化亚铁浓缩液在结晶釜中冷却得到四水合氯化亚铁晶体的浓缩液;经过自动离心机连续离心得到四水合氯化亚铁晶体;再经过输送机连续输送至气流干燥机进料斗;在四水合氯化亚铁通过进料斗的螺旋输送进入脉冲干燥塔;在温度为120~250℃、流速为20~50m/s的热空气中干燥脱水形成二水合氯化亚铁。该生产工艺的产能大、能耗低、操作清洁,生产的颗粒状产品质量稳定、不易结块、水溶性好,便于使用,达到土壤改良剂行业和饲料行业要求。 【EN】The invention discloses a production process of granular ferrous chloride dihydrate, which comprises the following steps: continuously feeding a ferrous chloride concentrated solution obtained by continuously evaporating and concentrating the ferrous chloride solution after filter pressing into a crystallization kettle with a jacket provided with cooling water at a discharge speed of 2-8 t/h for cooling; cooling the ferrous chloride concentrated solution in a crystallization kettle to obtain concentrated solution of ferrous chloride tetrahydrate crystals; continuously centrifuging by an automatic centrifuge to obtain ferrous chloride tetrahydrate crystals; then continuously conveying the mixture to a feed hopper of an air flow dryer by a conveyor; conveying ferrous chloride tetrahydrate into a pulse drying tower through a screw of a feed hopper; drying and dehydrating in hot air at the temperature of 120-250 ℃ and the flow rate of 20-50 m/s to form ferrous chloride dihydrate. The production process has the advantages of high capacity, low energy consumption, clean operation, stable quality of the produced granular product, difficult caking, good water solubility and convenient use, and meets the requirements of the soil conditioner industry and the feed industry.
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