WO2006066469A1 - Procédé de production d'un agent faisant fondre la neige à base d'acétate de calcium - Google Patents

Procédé de production d'un agent faisant fondre la neige à base d'acétate de calcium Download PDF

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Publication number
WO2006066469A1
WO2006066469A1 PCT/CN2005/000386 CN2005000386W WO2006066469A1 WO 2006066469 A1 WO2006066469 A1 WO 2006066469A1 CN 2005000386 W CN2005000386 W CN 2005000386W WO 2006066469 A1 WO2006066469 A1 WO 2006066469A1
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Prior art keywords
calcium acetate
wastewater
waste water
snow
melting agent
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PCT/CN2005/000386
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English (en)
French (fr)
Inventor
Guangjun Yu
Guoyi Zhu
Shuyi Zhang
Yanqiu Kou
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Changchun Jiachen Environment Protecting Equipment Co., Ltd
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Publication of WO2006066469A1 publication Critical patent/WO2006066469A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41—Preparation of salts of carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/18—Materials not provided for elsewhere for application to surfaces to minimize adherence of ice, mist or water thereto; Thawing or antifreeze materials for application to surfaces
    • C09K3/185—Thawing materials
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/02—Treatment of water, waste water, or sewage by heating
    • C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/048—Purification of waste water by evaporation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
    • C02F1/385—Treatment of water, waste water, or sewage by centrifugal separation by centrifuging suspensions
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/36—Organic compounds containing halogen
    • C02F2101/366—Dioxine; Furan
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds

Definitions

  • the invention belongs to a preparation method of a snow melting agent, in particular to a method for preparing calcium acetate.
  • furfural wastewater The demand for furfural and its downstream products is increasing rapidly. More than two hundred manufacturers are producing furfural.
  • the process is as follows: the corn cob is broken, steamed, dilute sulfuric acid is hydrolyzed, condensed to obtain a raw liquid, and then distilled by a distillation tower to obtain a crude aldehyde.
  • the distillation column is subjected to distillation, the bottom wastewater is produced, which is the main source of wastewater in the production of furfural, which is called furfural wastewater.
  • the invention provides a preparation method of calcium acetate snow melting agent, which solves the defects of high cost and long process flow in the preparation method of calcium acetate, and solves the problem of acetic acid pollution in furfural wastewater.
  • the technical solution adopted by the present invention is as follows: The following steps are included: 1. Neutralization of wastewater: The bottom wastewater generated in the production of furfural passes through a fluidized bed composed of limestone, and the contact time is 1 to 1.5 hours, so that the wastewater is neutralized to a pH of 7-8;
  • Residual liquid concentration The wastewater with neutralization PH value of 7 ⁇ 8 enters the double-effect evaporation system to evaporate the water in the wastewater, and the residual liquid is concentrated. When the solid content of the concentrated liquid is 40%, it is discharged; Filtration: The residual liquid discharged in the second step is transferred into the reaction vessel, and the powdered activated carbon having a weight of 10% to 15% is added, heated to boiling for 1 hour, adsorbed, centrifuged by a centrifuge, and the number of revolutions is 1800 to 1900 rpm. Filter
  • the invention has the advantages that: the acetic acid in the raw material is derived from the bottom wastewater in the production of furfural, and at the same time as the treatment, the calcium acetate is obtained, the waste water is recycled, and the sewage is discharged.
  • the cost of calcium acetate is greatly reduced. Even if the bottom wastewater in the production of furfural is treated, calcium acetate is obtained, and the purity is up to 92%, which fully meets the quality standard of the snow melting agent. The manufacturing cost of the snow melting agent is greatly reduced.
  • Residual liquid concentration The wastewater with neutralization PH value of 7 enters the double-effect evaporation system to evaporate the water in the wastewater, and the residual liquid is concentrated. When the solid content of the concentrated liquid is 40%, it is discharged; 3.
  • Adsorption filtration The residual liquid discharged in the second step is transferred into the reaction vessel, and 10% by weight of the powdered activated carbon is added, heated and boiled for 1 hour, adsorbed, centrifuged by a centrifuge, and rotated 1800/min, and filtered;
  • Wastewater Neutralization The bottom wastewater generated in the production of furfural passes through a fluidized bed composed of limestone. The contact time is 1.3 hours, and the wastewater is neutralized to a pH of 7.5.
  • Residual liquid concentration The wastewater with neutralization PH value of 7.5 enters the double-effect evaporation system to evaporate the water in the wastewater, and the residual liquid is concentrated. When the solid content of the concentrated liquid is 40%, it is discharged; 3. Adsorption filtration: The residual liquid discharged in the second step was transferred into the reaction vessel, and 12% by weight of powdered activated carbon was added thereto, and the mixture was heated and boiled for 1 hour, adsorbed, centrifuged by a centrifuge, and the number of revolutions was 1860/min.
  • Wastewater neutralization The bottom wastewater generated in the production of furfural passes through a fluidized bed composed of limestone, and the contact time is 1.5 hours, so that the wastewater is neutralized to a pH of 8;
  • Residual liquid concentration The wastewater with neutralization PH value of 8 enters the double-effect evaporation system to evaporate the water in the wastewater, and the residual liquid is concentrated. When the solid content of the concentrated liquid is 40%, it is discharged; 3. Adsorption filtration: The residual liquid discharged in the second step was transferred into the reaction vessel, and 15% by weight of the powdered activated carbon was added thereto, and the mixture was heated and boiled for 1 hour, adsorbed, centrifuged by a centrifuge, and rotated at 1900/min, and filtered;

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Hydrology & Water Resources (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Water Treatment By Sorption (AREA)
  • Removal Of Specific Substances (AREA)
  • Materials Applied To Surfaces To Minimize Adherence Of Mist Or Water (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Description

醋酸钙融雪剂的制备方法 技术领域
本发明属于一种融雪剂的制备方法，尤其是指一种醋酸钙的制备方 法。
背景技术
北方的冬季都需要大暈的融雪 来融化道路上的积雪， 目前许多融 雪剂都存在着污染环境、 融雪效果不佳、 融雪速度慢等缺点。 在各种融 雪剂中， 醋酸钙是较好的一种， 它对环境的污染程度低， 融雪效果好。 醋酸钙的制备通常是 ^^用醋酸和石灰石反应或是和氧化钙、氢氧化钙反 应， 该方法存在的缺点是成本高， 工艺流程长。 同时也增加了冬季城市 融雪的支出。玉米芯深加工生产糠醛始于上个世纪的三十年代， 我国于 五十年代引进， 全面发展的局面始于八十年代的后中期， 目前对糠醛及 其下游产品的需求迅速增加， 目前全国约有二百余个厂家在进行糠醛的 生产。 其工艺流程为： 将玉米芯破碎， 通入蒸汽、 稀硫酸水解， 冷凝， 得原液， 再用蒸馏塔进行蒸馏， 得粗醛。 蒸馏塔进行蒸馏时， 产生塔底 废水， 这也就是糠醛生产中主要的废水来源， 被称为糠醛废水。 一般年 产千吨的糠醛厂， 日糠醛废水排放量 100吨左右， COD在 15000~25000 之间， 约含 1.5〜2.5%的醋酸， 系污染物的主要物质， 如果没有有效的水 污染防治措施， 污染将相当严重。 .
发明内容
本发明提供一种醋酸钙融雪剂的制备方法， 以解决目前醋酸钙的制 备方法存在的成本高， 工艺流程长的缺点， 并且解决了糠醛废水中醋酸 的污染问题。 本发明采取的技术方案是： 包括下列步骤： 一、废水中和： 糠醛生产中的产生塔底废水经过一个由石灰石构成 的流化床， 接触时间为 1〜 1.5小时， 使该废水中和到 PH值 7~8；
二、 残液浓缩： 经中和 PH值为 7~8的废水进入双效蒸发系统， 使 废水中的水分蒸发，残液得到浓缩，当浓缩液固体含量为 40%时，排出； 三、吸附过滤： 将步骤二中排出的残液移入反应釜中， 加入其重量 10%〜15%的粉状活性炭， 加热至沸腾 1小时、 吸附， 用离心机离心， 转 数 1800~1900转 /分， 过滤；
四、 烘干滤液： 将步骤三中滤出液体烘干， 析出白色醋酸钙。
本发明的优点在于： 原料中醋酸来自糠醛生产中的塔底废水， 在对 其进行处理的同时， 得到醋酸钙， 使废水资源化， 污水零排放。 使醋酸 钙成本大大降低， 既使糠醛生产中的塔底废水得到了处理， 又得到了醋 酸钙， 纯度可达 92%， 完全符合融雪剂的质量标准。使融雪剂制造成本 大大降低。
具体实施方式
实施例 1
包括下列步骤：
一、废水中和： 糠醛生产中的产生塔底废水经过一个由石灰石构成 的流化床， 接触时间为 1小时， 使该废水中和到 PH值 7;
二、 残液浓缩： 经中和 PH值为 7的废水进入双效蒸发系统， 使废 水中的水分蒸发， 残液得到浓缩， 当浓縮液固体含量为 40%时， 排出； 三、 吸附过滤： 将步骤二中排出的残液移入反应釜中， 加入其重量 10%的粉状活性炭， 加热沸腾 1小时、吸附， 用离心机离心， 转数 1800/ 分， 过滤；
四、 烘干滤液： 将步骤三中滤出液体烘干， 析出白色醋酸钙。 实施例 2
包括下列步骤：
一、废水中和： 糠醛生产中的产生塔底废水经过一个由石灰石构成 的流化床， 接触时间为 1.3小时， 使该废水中和到 PH值 7.5 ;
二、 残液浓缩： 经中和 PH值为 7.5的废水进入双效蒸发系统， 使 废水中的水分蒸发，残液得到浓缩，当浓缩液固体含量为 40%时，排出； 三、 吸附过滤： 将步骤二中排出的残液移入反应釜中， 加入其重量 12%的粉状活性炭， 加热沸腾 1小时、吸附， 用离心机离心， 转数 1860/ 分， 过滤
四、 烘干滤液： 将步骤三中滤出液体烘干， 析出白色醋酸钙。
实施例 3
包括下列步骤- 一、废水中和： 糠醛生产中的产生塔底废水经过一个由石灰石构成 的流化床， 接触时间为 1.5小时， 使该废水中和到 PH值 8;
二、 残液浓缩： 经中和 PH值为 8的废水进入双效蒸发系统， 使废 水中的水分蒸发， 残液得到浓缩， 当浓缩液固体含量为 40%时， 排出； 三、 吸附过滤： 将步骤二中排出的残液移入反应釜中， 加入其重量 15%的粉状活性炭， 加热沸腾 1小时、吸附， 用离心机离心， 转数 1900/ 分， 过滤；
四、 烘干滤液： 将步骤三中滤出液体烘干， 析出白色醋酸钙。

Claims

权 利 要 求 书
1、 一种醋酸钙融雪剂的制备方法， 包括下列步骤- 一、废水中和： 糠醛生产中的产生塔底废水经过一个由石灰石构成 的流化床， 接触时间为 1~ 1.5小时， 使该废水中和到 PH值 7〜8；
二、 残液浓縮： 经中和 PH值为 7~8的废水进入双效蒸发系统， 使 废水中的水分蒸发，残液得到浓縮，当浓縮液固体含量为 40%时，排出； 三、 吸附过滤： 将步骤二中排出的残液移入反应釜中， 加入其重量 10%~15%的粉状活性炭， 加热沸腾 1小时、 吸附， 用离心机离心， 转数 1800〜1900转 /分， 过滤；
四、 烘干滤液： 将步骤三中滤出液体烘干， 析出白色醋酸钙。
PCT/CN2005/000386 2004-12-24 2005-03-28 Procédé de production d'un agent faisant fondre la neige à base d'acétate de calcium WO2006066469A1 (fr)

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CN102616871A (zh) * 2012-03-20 2012-08-01 蓝保(厦门)水处理科技有限公司 一种无机脱色水处理剂及其制备方法
KR101305589B1 (ko) 2011-02-28 2013-09-09 양정목 부산물 초산을 이용한 초산칼슘 제조방법 및 제조장치
CN112979452A (zh) * 2021-02-25 2021-06-18 上海第二工业大学 利用废弃液晶面板偏光膜热解气/油制备环保型醋酸钙融雪剂的方法
CN115594343A (zh) * 2022-10-18 2023-01-13 安徽金轩科技有限公司（Cn） 一种糠醛废水的处理方法

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CN102442793B (zh) * 2011-10-13 2013-08-07 大连理工大学 一种制砖材料的改性方法
CN102690632B (zh) * 2012-06-15 2014-05-14 天津喜研科技有限公司 一种木醋液制备环保融雪剂的方法
CN107021881A (zh) * 2016-12-27 2017-08-08 榆林职业技术学院 一种乙酸废液回收利用方法
CN106867454B (zh) * 2017-03-02 2018-10-12 辽宁科技学院 一种利用草木灰制备醋酸钾融雪剂的工艺
CN111471432A (zh) * 2020-04-03 2020-07-31 安徽科安废盐资源化有限公司 一种利用工业废杂盐制备融雪剂的方法

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KR101305589B1 (ko) 2011-02-28 2013-09-09 양정목 부산물 초산을 이용한 초산칼슘 제조방법 및 제조장치
CN102616871A (zh) * 2012-03-20 2012-08-01 蓝保(厦门)水处理科技有限公司 一种无机脱色水处理剂及其制备方法
CN112979452A (zh) * 2021-02-25 2021-06-18 上海第二工业大学 利用废弃液晶面板偏光膜热解气/油制备环保型醋酸钙融雪剂的方法
CN115594343A (zh) * 2022-10-18 2023-01-13 安徽金轩科技有限公司（Cn） 一种糠醛废水的处理方法

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