CN102974399A - Preparation method of catalytic cracking metal deactivator - Google Patents
Preparation method of catalytic cracking metal deactivator Download PDFInfo
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- CN102974399A CN102974399A CN2012105319279A CN201210531927A CN102974399A CN 102974399 A CN102974399 A CN 102974399A CN 2012105319279 A CN2012105319279 A CN 2012105319279A CN 201210531927 A CN201210531927 A CN 201210531927A CN 102974399 A CN102974399 A CN 102974399A
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Abstract
The invention discloses a preparation method of a catalytic cracking metal deactivator. The preparation method comprises the following steps of: (1) sequentially adding water, organic acid, triethylamine, ammonium hydrogen carbonate and antimony oxide to a reaction kettle, stirring uniformly so that the materials are fully dissolved, and simultaneously heating to 65-78 DEG C; (2) dropwise adding hydrogen peroxide to a mixed liquor obtained in the step (1) for carrying out oxidation reaction, wherein the reaction gives out heat, the mixture liquor reacts in boiling and continuously generates reflux, and the dropwise addition time is 30-45min; (3) heating for 20-40min after completing the dropwise addition of hydrogen peroxide, and maintaining a constant temperature of 103 DEG C; and (4) cooling and emptying to obtain the catalytic cracking metal deactivator. The preparation method has the advantages that the method is simple, and the used raw materials have low toxicity, no harm on human bodies, no secondary pollution on environments and no adverse effects on products and follow-up processing of the products.
Description
Technical field
The present invention relates to a kind of preparation method of catalytic cracking metal passivant.
Background technology
In catalytic cracking process, particularly in the catalytic cracking process take mink cell focus as raw material, the heavy metal that contains in the feedstock oil, catalyst surface be can be deposited on such as heavy metals such as nickel, vanadium, copper, iron and catalyst poisoning inactivation and selective decline caused, thereby yield of light oil is descended, and hydrogen and coke yield rise.Metallic pollution for catalytic cracking catalyst, industrial except raw material being carried out the demetalization preliminary treatment, selecting the strong catalyst of anti-metal ability, can also adopt the replacement rate that strengthens catalyst to improve the character of catalyst and the toxic action that suppresses the metal pair catalyst in the raw material with passivator.Wherein, using passivator is the simplest, effective method.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of catalytic cracking metal passivant.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of catalytic cracking metal passivant is characterized in that comprising the steps:
(1) water, organic acid, triethylamine, carbonic hydroammonium, antimony oxide are added reactor successively, stirring fully dissolves it, is warming up to simultaneously 65-78 ℃;
(2) drip hydrogen peroxide in the mixed liquor that obtains to step (1) and carry out oxidation reaction, exothermic heat of reaction, material reacts in boiling, and constantly produces and reflux, and time for adding is 30-45min;
(3) hydrogen peroxide dropwises, heating 20-40min, 103 ℃ of constant temperature;
(4) the cooling blowing obtains catalytic cracking metal passivant.
The parts by weight of each raw material of the present invention are: organic acid 7-9 part, triethylamine 22-27 part, hydrogen peroxide 140-160 part, antimony oxide 135-160 part, carbonic hydroammonium 30-40 part and water 160-180 part.
The parts by weight of each raw material of the present invention are preferably: 170 parts in 8 parts of organic acids, 25 parts of triethylamines, 150 parts in hydrogen peroxide, 150 parts of antimony oxides, 35 parts in carbonic hydroammonium and water.
Organic acid of the present invention is a kind of in sulfonic acid, sulfinic acid, tartaric acid, benzoic acid, the ascorbic acid.
Beneficial effect of the present invention: preparation method of the present invention is simple, and raw materials used toxicity is little, without injury, can not cause secondary pollution to environment to human body, and product and product following process are had no adverse effects.
The specific embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1
170 parts of water, 8 parts of tartaric acid, 25 parts of triethylamines, 35 parts of carbonic hydroammonium, 150 parts of antimony oxides are added reactor successively, and stirring fully dissolves it, is warming up to simultaneously 65-78 ℃, be added dropwise to again 150 parts of hydrogen peroxide and carry out oxidation reaction, exothermic heat of reaction, material reacts in boiling, and constantly produces backflow, time for adding 30-45min, hydrogen peroxide dropwises, and heating 20-40min keeps 103 ℃ of constant temperature, cool off at last blowing, obtain catalytic cracking metal passivant.Described catalytic cracking metal passivant is the yellow green supernatant liquid.The density (20 ℃) of measuring product with the described method of GB/T2504-81 is 1.15g/cm
3The kinematic viscosity of measuring product with the described method of GB/T265-88 is 3.8mm
2/ s; The freezing point of measuring product with the described method of GB/T510-83 is less than 10 ℃, and through the X-fluorescence spectrometer analysis, antimony content is 24% in the passivator.
Embodiment 2
165 parts of water, 7.2 parts of sulfonic acid, 23 parts of triethylamines, 33 parts of carbonic hydroammonium, 140 parts of antimony oxides are added reactor successively, and stirring fully dissolves it, is warming up to simultaneously 65-78 ℃, be added dropwise to again 155 parts of hydrogen peroxide and carry out oxidation reaction, exothermic heat of reaction, material reacts in boiling, and constantly produces backflow, time for adding 30-45min, hydrogen peroxide dropwises, and heating 20-40min keeps 103 ℃ of constant temperature, cool off at last blowing, obtain catalytic cracking metal passivant.Described catalytic cracking metal passivant is the yellow green supernatant liquid.The density (20 ℃) of measuring product with the described method of GB/T2504-81 is 1.32g/cm
3The kinematic viscosity of measuring product with the described method of GB/T265-88 is 4mm
2/ s; The freezing point of measuring product with the described method of GB/T510-83 is less than 10 ℃, and through the X-fluorescence spectrometer analysis, antimony content is 25% in the passivator.
Embodiment 3
175 parts of water, 7.8 parts of benzoic acid, 26 parts of triethylamines, 35 parts of carbonic hydroammonium, 145 parts of antimony oxides are added reactor successively, and stirring fully dissolves it, is warming up to simultaneously 65-78 ℃, be added dropwise to again 145 parts of hydrogen peroxide and carry out oxidation reaction, exothermic heat of reaction, material reacts in boiling, and constantly produces backflow, time for adding 30-45min, hydrogen peroxide dropwises, and heating 20-40min keeps 103 ℃ of constant temperature, cool off at last blowing, obtain catalytic cracking metal passivant.Described catalytic cracking metal passivant is the yellow green supernatant liquid.The density (20 ℃) of measuring product with the described method of GB/T2504-81 is 1.48g/cm
3The kinematic viscosity of measuring product with the described method of GB/T265-88 is 3.5mm
2/ s; The freezing point of measuring product with the described method of GB/T510-83 is less than 10 ℃, and through the X-fluorescence spectrometer analysis, antimony content is 23.5% in the passivator.
Embodiment 4
172 parts of water, 8.3 parts of ascorbic acid, 26.5 parts of triethylamines, 37 parts of carbonic hydroammonium, 135 parts of antimony oxides are added reactor successively, and stirring fully dissolves it, is warming up to simultaneously 65-78 ℃, be added dropwise to again 150 parts of hydrogen peroxide and carry out oxidation reaction, exothermic heat of reaction, material reacts in boiling, and constantly produces backflow, time for adding 30-45min, hydrogen peroxide dropwises, and heating 20-40min keeps 103 ℃ of constant temperature, cool off at last blowing, obtain catalytic cracking metal passivant.Described catalytic cracking metal passivant is the yellow green supernatant liquid.The density (20 ℃) of measuring product with the described method of GB/T2504-81 is 1.48g/cm
3The kinematic viscosity of measuring product with the described method of GB/T265-88 is 3.5mm
2/ s; The freezing point of measuring product with the described method of GB/T510-83 is less than 10 ℃, and through the X-fluorescence spectrometer analysis, antimony content is 24.2% in the passivator.
Embodiment 5
168 parts of water, 8 parts of ascorbic acid, 24 parts of triethylamines, 39 parts of carbonic hydroammonium, 156 parts of antimony oxides are added reactor successively, and stirring fully dissolves it, is warming up to simultaneously 65-78 ℃, be added dropwise to again 148 parts of hydrogen peroxide and carry out oxidation reaction, exothermic heat of reaction, material reacts in boiling, and constantly produces backflow, time for adding 30-45min, hydrogen peroxide dropwises, and heating 20-40min keeps 103 ℃ of constant temperature, cool off at last blowing, obtain catalytic cracking metal passivant.Described catalytic cracking metal passivant is the yellow green supernatant liquid.The density (20 ℃) of measuring product with the described method of GB/T2504-81 is 1.48g/cm
3The kinematic viscosity of measuring product with the described method of GB/T265-88 is 3.5mm
2/ s; The freezing point of measuring product with the described method of GB/T510-83 is less than 10 ℃, and through the X-fluorescence spectrometer analysis, antimony content is 24.2% in the passivator.
Embodiment 6
170 parts of water, 7.8 parts of ascorbic acid, 25 parts of triethylamines, 36 parts of carbonic hydroammonium, 155 parts of antimony oxides are added reactor successively, and stirring fully dissolves it, is warming up to simultaneously 65-78 ℃, be added dropwise to again 153 parts of hydrogen peroxide and carry out oxidation reaction, exothermic heat of reaction, material reacts in boiling, and constantly produces backflow, time for adding 30-45min, hydrogen peroxide dropwises, and heating 20-40min keeps 103 ℃ of constant temperature, cool off at last blowing, obtain catalytic cracking metal passivant.Described catalytic cracking metal passivant is the yellow green supernatant liquid.The density (20 ℃) of measuring product with the described method of GB/T2504-81 is 1.48g/cm
3The kinematic viscosity of measuring product with the described method of GB/T265-88 is 3.5mm
2/ s; The freezing point of measuring product with the described method of GB/T510-83 is less than 10 ℃, and through the X-fluorescence spectrometer analysis, antimony content is 24.2% in the passivator.
Following form is the passivation result data of Comparative Examples and embodiment under the same terms.
Table 1 is not for adding the passivation result of passivator in the Comparative Examples
Table 2 is for utilizing the passivation effect of the catalytic cracking metal passivant that the inventive method prepares
By table 1 and table 2 data as can be known, the matal deactivator of the present invention's preparation has good passivation effect.
Claims (4)
1. the preparation method of a catalytic cracking metal passivant is characterized in that comprising the steps:
(1) water, organic acid, triethylamine, carbonic hydroammonium, antimony oxide are added reactor successively, stirring fully dissolves it, is warming up to simultaneously 65-78 ℃;
(2) drip hydrogen peroxide in the mixed liquor that obtains to step (1) and carry out oxidation reaction, exothermic heat of reaction, material reacts in boiling, and constantly produces and reflux, and time for adding is 30-45min;
(3) hydrogen peroxide dropwises, heating 20-40min, 103 ℃ of constant temperature;
(4) the cooling blowing obtains catalytic cracking metal passivant.
2. the preparation method of catalytic cracking metal passivant according to claim 1 is characterized in that the parts by weight of each raw material are: organic acid 7-9 part, triethylamine 22-27 part, hydrogen peroxide 140-160 part, antimony oxide 135-160 part, carbonic hydroammonium 30-40 part and water 160-180 part.
3. the preparation method of catalytic cracking metal passivant according to claim 1 is characterized in that the parts by weight of each raw material are preferably: 170 parts in 8 parts of organic acids, 25 parts of triethylamines, 150 parts in hydrogen peroxide, 150 parts of antimony oxides, 35 parts in carbonic hydroammonium and water.
4. the preparation method of catalytic cracking metal passivant according to claim 1 is characterized in that described organic acid is a kind of in sulfonic acid, sulfinic acid, tartaric acid, benzoic acid, the ascorbic acid.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105778979A (en) * | 2014-12-22 | 2016-07-20 | 中国石油天然气股份有限公司 | Catalyst for reducing sulfur content of catalytically cracked gasoline and preparation method thereof |
| CN106475155A (en) * | 2015-08-28 | 2017-03-08 | 江苏科创石化有限公司 | A kind of matal deactivator and preparation method thereof |
| CN107159315A (en) * | 2017-05-27 | 2017-09-15 | 安徽卓远化工科技有限公司 | A kind of plant catalytic device many matal deactivators and preparation method thereof |
| CN107971041A (en) * | 2016-10-25 | 2018-05-01 | 中国石油化工股份有限公司 | A kind of preparation method of catalytic cracking metal passivant and the matal deactivator prepared by this method |
| CN107971042A (en) * | 2016-10-25 | 2018-05-01 | 中国石油化工股份有限公司 | A kind of preparation method of catalytic cracking metal passivant and the matal deactivator prepared by this method |
| CN107971040A (en) * | 2016-10-25 | 2018-05-01 | 中国石油化工股份有限公司 | A kind of preparation method of catalytic cracking metal passivant and the matal deactivator prepared by this method |
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| CN101885980A (en) * | 2010-07-26 | 2010-11-17 | 南京石油化工股份有限公司 | Preparation method and application of catalytic cracking metal passivant |
| CN102513163A (en) * | 2011-11-03 | 2012-06-27 | 山东京博控股股份有限公司 | Water-soluble catalytic cracking metal passivator and preparation method thereof |
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- 2012-12-11 CN CN2012105319279A patent/CN102974399A/en active Pending
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| CN101885980A (en) * | 2010-07-26 | 2010-11-17 | 南京石油化工股份有限公司 | Preparation method and application of catalytic cracking metal passivant |
| CN102513163A (en) * | 2011-11-03 | 2012-06-27 | 山东京博控股股份有限公司 | Water-soluble catalytic cracking metal passivator and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105778979A (en) * | 2014-12-22 | 2016-07-20 | 中国石油天然气股份有限公司 | Catalyst for reducing sulfur content of catalytically cracked gasoline and preparation method thereof |
| CN105778979B (en) * | 2014-12-22 | 2017-11-07 | 中国石油天然气股份有限公司 | A kind of catalyst for reducing sulfur content of catalytic cracking gasoline and preparation method thereof |
| CN106475155A (en) * | 2015-08-28 | 2017-03-08 | 江苏科创石化有限公司 | A kind of matal deactivator and preparation method thereof |
| CN106475155B (en) * | 2015-08-28 | 2019-09-20 | 江苏科创石化有限公司 | A kind of matal deactivator and preparation method thereof |
| CN107971041A (en) * | 2016-10-25 | 2018-05-01 | 中国石油化工股份有限公司 | A kind of preparation method of catalytic cracking metal passivant and the matal deactivator prepared by this method |
| CN107971042A (en) * | 2016-10-25 | 2018-05-01 | 中国石油化工股份有限公司 | A kind of preparation method of catalytic cracking metal passivant and the matal deactivator prepared by this method |
| CN107971040A (en) * | 2016-10-25 | 2018-05-01 | 中国石油化工股份有限公司 | A kind of preparation method of catalytic cracking metal passivant and the matal deactivator prepared by this method |
| CN107971040B (en) * | 2016-10-25 | 2020-09-18 | 中国石油化工股份有限公司 | Preparation method of catalytic cracking metal passivator and metal passivator prepared by same |
| CN107971041B (en) * | 2016-10-25 | 2020-09-22 | 中国石油化工股份有限公司 | Preparation method of catalytic cracking metal passivator and metal passivator prepared by same |
| CN107971042B (en) * | 2016-10-25 | 2020-09-22 | 中国石油化工股份有限公司 | Preparation method of catalytic cracking metal passivator and metal passivator prepared by same |
| CN107159315A (en) * | 2017-05-27 | 2017-09-15 | 安徽卓远化工科技有限公司 | A kind of plant catalytic device many matal deactivators and preparation method thereof |
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Application publication date: 20130320 |