KR930000095B1 - Process for manufacturing an inhibitors with a phosphorus-containing compounds - Google Patents
Process for manufacturing an inhibitors with a phosphorus-containing compounds Download PDFInfo
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- KR930000095B1 KR930000095B1 KR1019900011088A KR900011088A KR930000095B1 KR 930000095 B1 KR930000095 B1 KR 930000095B1 KR 1019900011088 A KR1019900011088 A KR 1019900011088A KR 900011088 A KR900011088 A KR 900011088A KR 930000095 B1 KR930000095 B1 KR 930000095B1
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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
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
- C02F5/02—Softening water by precipitation of the hardness
- C02F5/04—Softening water by precipitation of the hardness using phosphates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/18—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using inorganic inhibitors
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Abstract
Description
제1도는 본 발명의 방청제와 국내외 방청제의 부식실험결과를 나타낸 그래프.1 is a graph showing the corrosion test results of the rust inhibitors of the present invention and domestic and international rust inhibitors.
제2도는 본 발명의 방청제와 국내외 방청제의 용해속도 실험결과를 나타낸 그래프.2 is a graph showing the results of dissolution rate experiments of the rust inhibitors of the present invention and domestic and foreign rust inhibitors.
본 발명은 방청효과가 뛰어나고 다양한 용해속도를 나타내며 인체에 무해한 식수 및 공업용수용 중합인산염계 방청제의 제조방법에 관한 것이다.The present invention relates to a method for preparing a polymeric phosphate-based rust inhibitor for drinking water and industrial water which is excellent in rust prevention effect and shows various dissolution rates.
중합인산염계 방청제는 미국, 일본 등 선진각국에서 이미 수십년 전부터 연구개발하여 현재 상용화되고 있으며, 이에 대한 다수의 특허가 발표된 바 있다. 그중 몇가지 특허를 소개하면, 미국특허 3,284,368호에는 방청제의 용해 속도를 증가시키기 위하여 금속산화물과 P2O5의 몰비를 1.60 : 1-1.75 : 1로 하는 중합인산염계 방청제의 조성에 관하여 기재되어 있으며, 여기서 금속산화물로는 Na2O와 ZnO를 몰비 3.5 : 1-7:1로 사용하였다. 다른 미국특허 4,326,873호에는 액화탄화수소, 탄산소다, 금속산화물, 인산을 슬러리상태로 하여 고온중합로에서 800℃로 중합함으로써 물의 사용을 감소시키고 에너지를 절약하는 중합인산염계 방청제의 제조방법에 관하여 기재되어 있으며, 일본특허공보 소 49-9943호에는 인산칼슘 혹은 인산칼슘을 생성하는 인산과 칼슘화합물의 혼합물, 무수규산, 알칼리금속염의 혼합물을 백금도가니에서 온도 1200-1500℃로 3시간동안 고온중합하여 폴리인산칼슘 결합에 SiO2를 결합시켜 부식억제효과를 증가시키는 중합인산염계 방청제의 제조방법에 관하여 기재되어 있다.Polymeric phosphate-based rust inhibitors have been researched and developed for decades in advanced countries such as the United States and Japan, and are now commercially available. A number of patents have been published. Introducing several of them, US Pat. No. 3,284,368 describes the composition of a polymeric phosphate rust inhibitor having a molar ratio of metal oxide and P 2 O 5 of 1.60: 1-1.75: 1 to increase the dissolution rate of the rust inhibitor. In this case, Na 2 O and ZnO were used as the metal oxide in a molar ratio of 3.5: 1-7: 1. Other US Pat. No. 4,326,873 describes a method for producing a polymeric phosphate rust inhibitor which reduces the use of water and saves energy by polymerizing liquefied hydrocarbons, sodium carbonate, metal oxides and phosphoric acid in a slurry at 800 ° C. in a high temperature polymerization furnace. In Japanese Patent Publication No. 49-9943, a mixture of phosphoric acid and a calcium compound, calcium anhydride, and alkali metal salt, which is produced by calcium phosphate or calcium phosphate, is polymerized at a temperature of 1200-1500 ° C. in a platinum crucible for 3 hours. A method for preparing a polymerized phosphate rust preventive agent which increases the corrosion inhibitory effect by bonding SiO 2 to a calcium phosphate bond is described.
식수 및 공업용수용 중합인산염계 방청제는 방청효과가 뛰어나고 용도에 적합한 용해속도를 나타내며 인체에 무해하여야 한다.Polymeric phosphate anticorrosive for drinking water and industrial water has excellent anti-corrosive effect, shows dissolution rate suitable for the purpose, and should be harmless to human body.
본 발명에서는 제1인산소다 60-90wt%, 제2인산소다 0-10wt%, 탄산아연 0-20wt%, 산화아연 0-5wt%, 탄산칼슘 1-5wt%, 산화알루미늄 1-5wt%, 실리카 0-5wt%를 성분으로 하는 중합인산염계 방청제를 개발함으로써 방청효과가 뛰어나고 다양한 용해속도를 나타내며 뿐만 아니라 인체에 무해한 식수 및 공업용수용 중합인산염계 방청제를 저가로 생산할 수 있게 되었다. 제1인산소다는 중합인산염 방청제의 주성분으로 60-90wt%가 되어야 방청효과 및 방청제의 결합력을 유지시킬 수 있다. 제2인산소다는 방청제의 용해 속도를 증가시키기 위한 것으로 제2인산소다의 양을 증가시킬수록 용해속도가 증가하나 10wt%이상에서는 용해속도의 증가효과가 미미하므로 0-10wt%의 조성비가 적당하다.In the present invention, the first sodium phosphate 60-90wt%, the second sodium phosphate 0-10wt%, zinc carbonate 0-20wt%, zinc oxide 0-5wt%, calcium carbonate 1-5wt%, aluminum oxide 1-5wt%, silica By developing a polymerized phosphate rust inhibitor comprising 0-5wt%, it is excellent in rust prevention effect and shows various dissolution rates, and it is possible to produce polymerized phosphate rust inhibitor for drinking water and industrial water which is harmless to human body. Sodium primary phosphate should be 60-90wt% as the main component of the polymerized phosphate rust inhibitor to maintain the rust preventive effect and binding strength of the rust inhibitor. Sodium diphosphate increases the dissolution rate of the rust preventive agent. As the amount of dibasic sodium phosphate increases, the dissolution rate increases, but the increase rate of dissolution rate is less than 10wt%. .
탄산아연 및 산화아연은 방청제의 방청효과를 증가시키기 위한 것으로 단독 혹은 혼합하여 사용할 수 있다. 탄산아연인 경우는 20wt%이상, 산화아연인 경우는 5wt%이상 초과하면 방청효과가 증가하지 않는다. 따라서 적절한 조성비는 탄산아연 0-20wt%, 산화아연 0-5wt%이며, 두화합물을 혼합하여 사용할 시는 두화합물의 무게합이 20wt%를 넘지 않도록 하여야 한다. 탄산칼슘은 중합인산염 방청제의 주성분으로 용해속도에 영향을 미치는데 5wt%로 이상에서는 용해속도의 증가효과가 미미하므로 1-5wt%로 하는 것이 바람직하다.Zinc carbonate and zinc oxide are used to increase the rust prevention effect of the rust preventive agent and may be used alone or in combination. If zinc carbonate is more than 20wt%, and zinc oxide is more than 5wt%, the antirust effect does not increase. Therefore, the proper composition ratio is 0-20wt% zinc carbonate and 0-5wt% zinc oxide, and when the two compounds are mixed, the sum of the two compounds should not exceed 20wt%. Calcium carbonate is the main component of the polymerized phosphate rust inhibitor, which affects the dissolution rate. Since the increase effect of dissolution rate is insignificant above 5 wt%, it is preferable to set it as 1-5 wt%.
산화알루미늄은 중합인산염의 결합력을 증가시켜 성형과정에서의 성형화가 잘 이루어지도록 하는 것으로 5wt%이상에서는 그 용해속도의 증가효과가 미미하므로 1-5wt%의 조성비를 사용하는 것이 바람직하다. 실리카는 중합인산염의 방청효과를 증가시키기 위한 것으로 5wt%이상에서는 방청효과 증가가 뚜렷하지 않기 때문에 0-5wt%의 조성비가 적당하다.Aluminum oxide is to increase the binding force of the polymerized phosphate to make the molding well in the molding process, and the increase in dissolution rate is less than 5wt%, it is preferable to use a composition ratio of 1-5wt%. Silica is intended to increase the rust prevention effect of the polymerized phosphate, and the composition ratio of 0-5wt% is suitable because the increase in the rust prevention effect is not obvious at 5wt% or more.
본 발명의 중합인산염계 방청제의 제조공정을 자세히 설명하면 다음과 같다.Referring to the manufacturing process of the polymerized phosphate-based rust inhibitor of the present invention in detail.
우선 제1인산소다, 제2인산소다, 탄산아연, 산화아연, 탄산칼슘, 산화알루미늄, 실리카의 해당량을 균일하게 혼합하여 건조기에 넣고 약 120℃에서 1시간 건조, 탈수시킨다.First, the corresponding amounts of the first sodium phosphate, the second sodium phosphate, zinc carbonate, zinc oxide, calcium carbonate, aluminum oxide, and silica are mixed uniformly, placed in a drier, and dried and dehydrated at about 120 ° C. for 1 hour.
건조, 탈수된 고체시료를 알루미나 도가니에 넣은 후 전기로에 넣고 가열속도 10℃/min로 850℃까지 가열하여 고체시료를 용융시킨다. 용융된 시료 -850℃에서 1시간 유지하여 중합시킨다. 중합은 xNa2OyP2O5형태의 고분자 인산염을 만드는 것을 의미하는데, 중합온도 및 중합시간에 따라 x/y의 비가 변하게 되며 그 비는 1-2가 적당하다.The dried and dehydrated solid sample is placed in an alumina crucible and placed in an electric furnace to heat the solid sample to 850 ° C. at a heating rate of 10 ° C./min. The molten sample is kept at -850 ° C for 1 hour to polymerize. Polymerization refers to making a polymer phosphate of xNa 2 OyP 2 O 5 form, the ratio of x / y changes depending on the polymerization temperature and polymerization time, the ratio is suitable 1-2.
중합온도가 높을수록 동일한 중합도를 얻기위한 중합시간을 짧게 할 수 있으며, 적절한 중합온도는 800-1000℃, 중합시간은 30분-1시간이다. 중합된 인산염은 미리 200℃로 예열한 성형기에 넣어 성형함으로써 무색 투명한 유리형태의 중합인산염계 방청제를 제조한다.The higher the polymerization temperature, the shorter the polymerization time to obtain the same degree of polymerization, the suitable polymerization temperature is 800-1000 ℃, the polymerization time is 30 minutes-1 hours. The polymerized phosphate is put into a molding machine preheated to 200 ° C. to prepare a polymerized phosphate rust inhibitor in the form of colorless transparent glass.
[실시예]EXAMPLE
시료의 조성을 아래의 표1과 같이하여 균일하게 혼합한 후 건조기에서 약 120℃로 1시간 정도 건조·탈수시킨다.The composition of the sample is mixed as shown in Table 1 below, and then dried and dehydrated at about 120 ° C. for 1 hour in a dryer.
건조, 탈수된 상기의 시료를 알루미나 도가니에 넣고 전기로에 넣은후 가열속도 10℃/min로 850℃까지 가열하여 용융시킨다.The dried and dehydrated samples are placed in an alumina crucible, placed in an electric furnace, and heated to melt at 850 ° C. at a heating rate of 10 ° C./min.
용융된 시료를 850℃에서 1시간 유지함으로서 중합시키고, 이 중합인산염을 미리 200℃로 예열한 성형기에 넣어 성형함으로써 무색 투명한 유리형태의 중합인산염계 방청제를 제조한다.The molten sample is kept at 850 ° C. for 1 hour to polymerize, and the polymerized phosphate is put into a molding machine preheated to 200 ° C. in advance to prepare a colorless transparent glass polymer phosphate rust inhibitor.
[표 1]TABLE 1
상기의 방법으로 제조한 중합인산염계 방청제를 원자 흡수법에 의하여 중금속을 분석한 결과 표 2와 같이 나타났다.As a result of analyzing the heavy metal of the polymerized phosphate-based rust inhibitor prepared by the above method by the atomic absorption method, it was shown in Table 2.
표에서 보는 바와 같이 중금속양이 보건사회부의 위생 1435-호(1984년) 급수용 방청제 사용에 관한 지도, 감독지침의 기준허용치보다 훨씬 낮은 양으로 나타나 거의 인체에 무해한 방청제로 판명되었다.As shown in the table, the amount of heavy metals was found to be almost harmless to humans because it was much lower than the standard allowance in the guidelines and supervision guidelines for sanitation 1435- (1984) of the Ministry of Health and Social Affairs.
[표 2]TABLE 2
본 발명의 중합인산염계 방청제의 방청효과(부식억제효과)를 현재 시판되고 있는 외국산방청제(상표명:Siliphos)와 국산방청제에 대하여 방청제가 용해된 용액에서 탄소강시편의 전기화적 전류-전위 분극곡선으로부터 부식속도를 계산하는 분극실험으로 부식속도를 측정하여 비교한 결과 제1도와 같이 나타났다. 도면으로 부터 알 수 있듯이 본 발명의 방청제는 외국산 Siliphos와 시중의 국산방청제보다 훨씬 낮은 부식속도를 나타냈는데 이로써 본 발명의 방청제의 방청효과(부식억제효과)가 다른 제품보다 훨씬 우수하다는 사실이 입증된 것이다.Corrosion effect (corrosion inhibitory effect) of the polymerized phosphate-based rust inhibitor of the present invention is corroded from electrochemical current-potential polarization curves of carbon steel specimens in a solution in which a rust inhibitor is dissolved in foreign commercial rust inhibitors (trade name: Siliphos) and domestic rust inhibitors. In the polarization test to calculate the rate, the corrosion rate was measured and shown in FIG. As can be seen from the drawings, the anti-corrosive agent of the present invention exhibited a much lower corrosion rate than that of foreign-type Siliphos and commercially available domestic anti-corrosive agent, which proved that the anti-corrosive effect (corrosion inhibitory effect) of the anti-corrosive agent of the present invention was much superior to other products. will be.
제2도는 본 발명의 방청제 및 시판되고 있는 국내외 방청제의 용해속도를 비교 실험한 결과이다. 용해도는 방청제 10g이 증류수 200ml 중에 시간이 경과함에 따라 용해되는 양을 측정한 것으로 본 발명의 방청제는 다양한 용해속도를 나타내는 것을 알 수 있다.2 is a result of a comparative experiment of the dissolution rate of the rust inhibitor of the present invention and commercially available rust inhibitors at home and abroad. The solubility was measured by measuring the amount of 10 g of the rust preventive agent dissolved over time in 200 ml of distilled water, and it can be seen that the rust preventive agent of the present invention exhibits various dissolution rates.
특히 실시예3의 용해도 실험결과로 알 수 있듯이 본 발명에서는 제2인산소다를 소량 첨가함으로써 용해속도를 증가시켰는데 이는 사용자의 용도에 적합한 용해속도를 가진 방청제를 제2인산소다의 양으로 조정하여 제조할 수 있다는 것을 나타내 준다.In particular, as can be seen from the solubility test result of Example 3, in the present invention, the dissolution rate was increased by adding a small amount of dibasic sodium phosphate, which was adjusted to the amount of dibasic sodium phosphate having a dissolution rate suitable for the user's use. It can be produced.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109338369A (en) * | 2018-10-29 | 2019-02-15 | 万玉梅 | A kind of preparation method of composition metal corrosion inhibiter |
| RU2763494C1 (en) * | 2020-10-26 | 2021-12-29 | Федеральное государственное бюджетное образовательное учреждение высшего образования «Магнитогорский государственный технический университет им. Г.И. Носова», | Composition for treating makeup water in centralised heat supply systems |
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1990
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109338369A (en) * | 2018-10-29 | 2019-02-15 | 万玉梅 | A kind of preparation method of composition metal corrosion inhibiter |
| RU2763494C1 (en) * | 2020-10-26 | 2021-12-29 | Федеральное государственное бюджетное образовательное учреждение высшего образования «Магнитогорский государственный технический университет им. Г.И. Носова», | Composition for treating makeup water in centralised heat supply systems |
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