CN1008809B - Method for producing lead hydroxide - Google Patents
Method for producing lead hydroxideInfo
- Publication number
- CN1008809B CN1008809B CN 85105914 CN85105914A CN1008809B CN 1008809 B CN1008809 B CN 1008809B CN 85105914 CN85105914 CN 85105914 CN 85105914 A CN85105914 A CN 85105914A CN 1008809 B CN1008809 B CN 1008809B
- Authority
- CN
- China
- Prior art keywords
- lead
- acetate
- weight
- hydroxide
- concentration
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 229910021514 lead(II) hydroxide Inorganic materials 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title abstract description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229940046892 lead acetate Drugs 0.000 claims abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims abstract description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 15
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 8
- 239000005695 Ammonium acetate Substances 0.000 claims description 8
- 229940043376 ammonium acetate Drugs 0.000 claims description 8
- 235000019257 ammonium acetate Nutrition 0.000 claims description 8
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 11
- 239000003381 stabilizer Substances 0.000 description 8
- OCWMFVJKFWXKNZ-UHFFFAOYSA-L lead(2+);oxygen(2-);sulfate Chemical compound [O-2].[O-2].[O-2].[Pb+2].[Pb+2].[Pb+2].[Pb+2].[O-]S([O-])(=O)=O OCWMFVJKFWXKNZ-UHFFFAOYSA-L 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 229910000464 lead oxide Inorganic materials 0.000 description 5
- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 description 4
- 239000004135 Bone phosphate Substances 0.000 description 4
- 229920000915 polyvinyl chloride Polymers 0.000 description 4
- 239000004800 polyvinyl chloride Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000012716 precipitator Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- PNZVFASWDSMJER-UHFFFAOYSA-N acetic acid;lead Chemical compound [Pb].CC(O)=O PNZVFASWDSMJER-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- UQLDLKMNUJERMK-UHFFFAOYSA-L di(octadecanoyloxy)lead Chemical compound [Pb+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O UQLDLKMNUJERMK-UHFFFAOYSA-L 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002611 lead compounds Chemical class 0.000 description 1
- YJOMWQQKPKLUBO-UHFFFAOYSA-L lead(2+);phthalate Chemical compound [Pb+2].[O-]C(=O)C1=CC=CC=C1C([O-])=O YJOMWQQKPKLUBO-UHFFFAOYSA-L 0.000 description 1
- UMKARVFXJJITLN-UHFFFAOYSA-N lead;phosphorous acid Chemical compound [Pb].OP(O)O UMKARVFXJJITLN-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
本发明是有关生产二价氢氧化铅的方法，这种二价氢氧化铅在商业上可用作生成所有铅化合物的原料。This invention relates to a process for the production of divalent lead hydroxide which is commercially available as a starting material for all lead compounds.
尤其是这些氢氧化铅在塑料工业中，用来生产耐热及耐紫外线、降解聚氯乙烯树脂的稳定剂。典型的衍生物有三盐基硫酸铅、四价盐基硫酸铅、硅硫酸铅、二盐基亚磷酸铅、邻苯二甲酸铅、二盐基硬脂酸铅和硬脂酸铅。In particular, these lead hydroxides are used in the plastics industry to produce heat-resistant and UV-resistant stabilizers that degrade polyvinyl chloride resins. Typical derivatives are tribasic lead sulfate, tetrabasic lead sulfate, lead silicosulfate, dibasic lead phosphite, lead phthalate, dibasic lead stearate and lead stearate.
氢氧化铅也用于涂料和颜料工业中。Lead hydroxide is also used in the paint and pigment industry.
上述提到的稳定剂，目前是采用这样一种工艺生产的，这种方法是在很高温度下，把空气吹进熔化了的铅来生产氧化铅。这样生产出的氧化铅，在控制一定的条件下和水，然后和硫酸制成泥浆状，使得三盐基硫酸铅沉淀出来。分离出这沉淀物并使之干燥，以作为稳定剂使用。现已发现这种生产方法造成严重的大气污染，并且最终产品中含有未反应掉的铅的浓度太高。例如美国专利第3，323，859号中聚氯乙烯树脂的二盐基铅盐稳定剂的生产采用氧化铅低浓乙酸的反应，接着将由此生成的二盐基乙酸铅再和硫酸钠反应。The aforementioned stabilizers are currently produced by a process in which air is blown into molten lead at very high temperatures to produce lead oxide. The lead oxide produced in this way is mixed with water under certain conditions, and then mixed with sulfuric acid to make a slurry, so that tribasic lead sulfate is precipitated. The precipitate was separated and dried for use as a stabilizer. It has been found that this production method causes severe atmospheric pollution and the final product contains too high a concentration of unreacted lead. For example U.S. Patent No. 3,323, the production of the dibasic lead salt stabilizer of polyvinyl chloride resin adopts the reaction of lead oxide low concentrated acetic acid in No. 859, then the dibasic lead acetate generated thus is reacted with sodium sulfate again.
曾经采取过许多处理办法来避免在稳定剂的生产中使用氧化铅。美国专利第452，386号将金属铅经过低浓乙酸及空气的交替作用转变成乙酸铅，然后将乙酸铅和硫酸进行反应。Numerous approaches have been taken to avoid the use of lead oxide in the production of stabilizers. U.S. Patent No. 452, No. 386, metal lead is converted into lead acetate through the alternation of low-concentration acetic acid and air, and then lead acetate and sulfuric acid are reacted.
本发明的主要目的是提出生产二价氢氧化铅的方法，这种方法把污染减少到最低限度并且制得这样的一种产品，这种产品可以应用在涂料和颜料工业中，本方法还避免了在生产聚氯乙烯树脂稳定剂中使用氧化 铅。The main object of the present invention is to propose a method for the production of divalent lead hydroxide which minimizes pollution and produces a product which can be used in the paint and pigment industry, which also avoids the In order to use oxidation in the production of polyvinyl chloride resin stabilizers lead.
因此，提出一种生产二价氢氧化铅的方法，其特征在于采用如下步骤，（1）将金属铅在不超过200℃和在绝对压力为1至10大气压的含氧气氛中和乙酸反应形成乙酸铅，然后（2）将乙酸铅和一铵离子物料在温度不超过100℃、绝对压力为1到5大气压下反应生成沉淀的氢氧化铅。Therefore, a method for producing divalent lead hydroxide is proposed, which is characterized in that the following steps are adopted: (1) reacting metallic lead with acetic acid at no more than 200° C. and in an oxygen-containing atmosphere with an absolute pressure of 1 to 10 atmospheres to form lead acetate, and then (2) react lead acetate and monoammonium ion material at a temperature not exceeding 100°C and an absolute pressure of 1 to 5 atmospheres to form precipitated lead hydroxide.
乙酸浓度可低于50%（重量），最好低于25%（重量）;如果以乙酸铵状态加入，则其浓度应低于50%（重量），最好低于35%（重量）。The concentration of acetic acid may be less than 50% by weight, preferably less than 25% by weight; if added in the form of ammonium acetate, the concentration should be less than 50% by weight, preferably less than 35% by weight.
下述实例公开了本项发明的一种方案，并附有一张流程图来说明以下工序：Following example discloses a kind of scheme of the present invention, and a flow chart is attached to illustrate following operation:
实例1Example 1
乙酸铵水溶液按重量计浓度为35%，于温度100℃时在一通氧的密闭容器中和过量金属铅反应1个小时。乙酸铵分解，生成的乙酸在绝对压力为5大气压的氧气氛下和铅反应生成乙酸铅溶液和氨。The ammonium acetate aqueous solution has a concentration of 35% by weight, and reacts with excess metal lead in an airtight container with oxygen at a temperature of 100°C for 1 hour. Ammonium acetate decomposes, and the acetic acid of generation reacts with lead to generate lead acetate solution and ammonia under the oxygen atmosphere of 5 atmospheres of absolute pressure.
将氨带出来并经压缩，而氧气流回到反应器。The ammonia is brought out and compressed, while the oxygen flows back to the reactor.
将乙酸铅水溶液的温度调节至80℃并且送至沉淀器，再通入氨气，包括前一步回收得到的氨，直至压力达到3个大气压绝对值为止。于是，氢氧化铅沉淀出来，生成乙酸铵溶液。Adjust the temperature of the lead acetate aqueous solution to 80°C and send it to the precipitator, and then feed ammonia gas, including the ammonia recovered in the previous step, until the pressure reaches an absolute value of 3 atmospheres. Then, lead hydroxide precipitates out, generating ammonium acetate solution.
实例2Example 2
该实例介绍了制备二盐基和三盐基硫酸铅的方法，但该实例并不成为所要求保护的发明部分。它只是一个简单的实施例，介绍如何使用氢氧化铅作为初始反应物，以生产其它许多含铅化合物，例如三盐基和四盐基硫酸铅。本文所用的三盐基和四盐基硫酸铅的表达如下：This example describes the preparation of dibasic and tribasic lead sulfates, but this example does not form part of the claimed invention. It is just a simple example of how to use lead hydroxide as an initial reactant to produce many other lead-containing compounds such as tribasic and tetrabasic lead sulfate. The expressions tribasic and tetrabasic lead sulfate used herein are as follows:
3PbO·pbSO4·H2O 三盐基硫酸铅3PbO·pbSO 4 ·H 2 O tribasic lead sulfate
4PbO·PbSO4四盐基硫酸铅4PbO·PbSO 4 tetrabasic lead sulfate
进行与实例1所公开的工序相同的工序。The same procedure as that disclosed in Example 1 was carried out.
在沉淀器中将按化学比计量的硫酸和实例1中的氢氧化铅反应，由 此氢氧化铅转换成三盐基硫酸铅沉淀物。将这种分散在液体中的沉淀物分离出来并进行干燥。铅进料83.6公斤，所获之干燥三盐基硫酸铅产量是100公斤。In the precipitator, the sulfuric acid metered by stoichiometry and the lead hydroxide in the example 1 are reacted, by This lead hydroxide is converted to lead sulfate tribasic precipitate. This precipitate dispersed in the liquid is separated and dried. Lead feed 83.6 kilograms, the obtained dry tribasic lead sulfate output is 100 kilograms.
所获之固体掺加到聚氯乙烯树脂内作为稳定剂来使用，然后这固体通过挤压机制成试样。液体在一汽提循环中加热，使所有溶解的氨逸出，再将氨回收作重复使用，乙酸铵的浓度按重量计调整为35%。然后将它通到反应器中，使之与新的一批金属铅一起进料重复进行流程的第一步反应。The obtained solid was added to polyvinyl chloride resin as a stabilizer, and then the solid was passed through an extrusion machine to form a test piece. The liquid is heated in a stripping cycle to allow all dissolved ammonia to escape and the ammonia is recovered for reuse. The ammonium acetate concentration is adjusted to 35% by weight. It is then passed to the reactor to be fed with a new batch of metallic lead to repeat the first step of the process.
与用相同的树脂和市售稳定剂制成的同类试样相比，本发明方法提供的试样被认为具有更有效的稳定作用，同时没有损害对树脂所要求的性质。另外，由本发明方法所得之三盐基硫酸铅基本上不含有（低于5ppm）单质铅、单盐基硫酸铅和未反应的氧化铅。The method of the present invention provides samples that are believed to have more effective stabilization than comparable samples made with the same resin and commercially available stabilizers, without compromising the desired properties of the resin. In addition, the tribasic lead sulfate obtained by the method of the present invention basically does not contain (less than 5 ppm) elemental lead, monobasic lead sulfate and unreacted lead oxide.
还要注意到本发明方法控制在中等温度和压力下操作，这样设备需用的投资费用比通常工艺所需要的要低得多，并且操作费用也比较低。Note also that the process of the present invention is controlled to operate at moderate temperatures and pressures so that capital costs for equipment are much lower than those required by conventional processes, and operating costs are also relatively low.
Claims (6)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85105914 CN1008809B (en) | 1985-08-05 | 1985-08-05 | Method for producing lead hydroxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85105914 CN1008809B (en) | 1985-08-05 | 1985-08-05 | Method for producing lead hydroxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85105914A CN85105914A (en) | 1987-02-25 |
| CN1008809B true CN1008809B (en) | 1990-07-18 |
Family
ID=4794771
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 85105914 Expired CN1008809B (en) | 1985-08-05 | 1985-08-05 | Method for producing lead hydroxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1008809B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104961155A (en) * | 2015-05-29 | 2015-10-07 | 超威电源有限公司 | Method for preparing lead oxide by using lead-acid storage battery positive electrode plate coating waste lead paste |
| CN104961154A (en) * | 2015-05-29 | 2015-10-07 | 超威电源有限公司 | Method for preparing lead oxide by using lead-acid storage battery positive electrode acid leaching waste lead mud |
-
1985
- 1985-08-05 CN CN 85105914 patent/CN1008809B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN85105914A (en) | 1987-02-25 |
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