CN105087068A - Process for preparing oxidized wax from coal wax - Google Patents
Process for preparing oxidized wax from coal wax Download PDFInfo
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- CN105087068A CN105087068A CN201510582254.3A CN201510582254A CN105087068A CN 105087068 A CN105087068 A CN 105087068A CN 201510582254 A CN201510582254 A CN 201510582254A CN 105087068 A CN105087068 A CN 105087068A
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Abstract
The invention relates to a process for preparing oxidized wax from coal wax. The process comprises the following steps of preparing for a raw material, namely F-T coal wax, adding F-T coal wax into a three-neck flask, gradually heating to 100 DEG C and melting the F-T coal wax; then, adding a catalyst, wherein the weight of the catalyst accounts for 0.1-1.0% of the weight of the F-T coal wax; and introducing 0.2-0.8L/h oxygen gas to each gram of F-T coal wax, controlling the reaction temperature within 125-160 DEG C at the stage, reacting for 3-8 hours, then, taking out the product while the product is hot, sampling and analyzing. According to the process, the oxidized wax is prepared from the F-T coal wax instead of the traditional wax, so that the burden of petroleum resource shortage is relieved, and the economic additional value of the coal wax is increased; materials such as a heavy metal ionic catalyst, nitrogen shielding gases, a water-carrying agent and polymerization additives are not used; the reaction time is short, the process is simple and convenient to operate, the prepared oxidized wax product is light in color and smell, and the acid value and saponification value of the prepared oxidized wax product meet the requirements of the SASOLWAX A28 index of south Africa; and no special processing equipment is required in the process.
Description
Technical field
The present invention relates to the preparation field of oxidized petroleum waves, the technique of the waxed standby oxidized petroleum waves of especially a kind of matchmaker.
Background technology
Wax has purposes widely at rubber and plastic industry, coating, ink area and daily chemical industry.Wax is through oxidation modification in various degree, its long linear is brought hydroxyl, carboxyl, ester group group and be provided with certain polarity, better consistency is had with fluoropolymer resin, organic-inorganic color stuffing, can emulsification in water, thus expand the range of application of wax.
Wax can comprise paraffin, Microcrystalline Wax, Fischer-Tropsch wax, polyethylene wax, Poly Propylene Wax etc.The index of the degree of oxidation of wax can be the acid number of the oxidation products of wax, and the KOH milligram number namely and needed for 1 gram of (g) sample, represents with mgKOH/g.Oxidized petroleum waves as the inside and outside lubricant agent of PVC processing, filling master batch and the Ricinate of colour batch, the brightening agent of rubber etc., can may be used for preparing wax emulsion and daily chemical products, also can be processed as saponification, esterified wax further usually.
CN104178219A discloses a kind of method that Microcrystalline Wax produced by F-T synthesis waxy stone; wherein disclose: along with the day by day exhausted of world petroleum resource and the continuous enhancing to environmental protection consciousness, research and the substitute finding eco-friendly petroleum-based energy become one of direction that world-technology develops.Prepare coal wax with coal and Sweet natural gas by F-T synthesis (Fischer-TropschSynthesis) reaction and replace prior paraffin, one side can solve petroleum resources shortage problem, meets national economy and increases demand to the energy fast; The economic value added of Fischer-Tropsch wax can be improved on the other hand, the environmental pollution caused of directly burning can also be reduced simultaneously, significant.
Document [the development and application of paraffin oxidation modification, Liaoning chemical industry, 2009,38 (9): 670 ~ 673] disclose: in recent years, although China makes some progress in exploitation oxidized petroleum waves, there is some deficiency following: do not form large-scale exploitation, production and application situation; Oxidized petroleum waves color is dark, smell is heavy, second-rate; The index such as acid number, saponification value can not meet demand, limits it and uses; Containing impurity such as the friendship matter that remaining catalyzer and reaction generate.
CN103468316A discloses a kind of preparation method of peracid soap oxidized petroleum waves, disclose the method using manganese salt (manganous sulfate) as catalyst preparing oxidized petroleum waves, although this product acid number reaches 23.71mgKOH/g, saponification value reaches 49.13mgKOH/g, but in oxygen atmosphere, metal ion can oxidized production metal oxide and other by products, deepen coloured product, reduce catalyst activity.
CN1206719A discloses a kind of method of Alathon of being prepared by metalloscene catalyst by oxygen or oxygenous gaseous mixture melt oxidation and copolymer waxes, the acid number 18.00mgKOH/g of its oxidized petroleum waves prepared, saponification value 40mgKOH/g.
The method of hardening oxidation wax is produced under a kind of nitrogen protection condition reported by document [development of hardening oxidation wax, petrochemical technology and application .2007,25 (4): 314 ~ 315];
CN101289540A, CN101724107A all disclose the method for oxidation of polyethylene wax or ethylene waxes emulsion.
From above-mentioned publication and document, there is the report about F-T wax synthesis Microcrystalline Wax, paraffin oxidation, polyethylene wax oxidation, but the report also not having F-T coal wax to be oxidized both at home and abroad so far, and its correlative study direction value obtains further investigated.
Summary of the invention
The technical problem to be solved in the present invention is: propose to substitute with F-T coal wax the novel process that prior paraffin prepares oxidized petroleum waves.
The technical solution adopted in the present invention is: the technique of the waxed standby oxidized petroleum waves of a kind of matchmaker, comprises the steps:
A () prepares raw material F-T coal wax, and add in there-necked flask, is warming up to 100 DEG C gradually and makes it melt;
B () adds the catalyzer that weight is 0.1% ~ 1.0% of F-T coal wax again;
C () passes into the oxygen of 0.2 ~ 0.8L/h according to each gram of F-T coal wax, this elementary reaction temperature controls at 125 DEG C ~ 160 DEG C, after reaction 3 ~ 8h, takes out product while hot and sampling analysis.
Further, as a kind of concrete embodiment, catalyzer described in the present invention is any in stearic acid, boric acid, tosic acid, or combinations several arbitrarily.
Further, as a kind of concrete embodiment, the weight of catalyzer described in the present invention is 0.5% of F-T coal wax
The invention has the beneficial effects as follows: mainly contain following some:
(1) substitute prior paraffin with F-T coal wax and prepare oxidized petroleum waves, alleviate the pressure of petroleum resources shortage, improve the economic value added of coal wax;
(2) this technique does not adopt the materials such as heavy metal ion catalyzer, nitrogen protection gas, water entrainer and reagent and additive in polymerization;
(3) this technological reaction time is short, easy and simple to handle, and the oxidized petroleum waves product color of preparation is shallow, and smell is light, and acid number, saponification value all reach South Africa SASOLWAXA28 index request;
(4) this technique does not need special processing units.
Embodiment
The present invention is further detailed explanation in conjunction with the preferred embodiments now.
Embodiment 1
40g coal wax is added in the there-necked flask of 500mL that thermometer, inlet pipe and offgas duct are housed, heat up fusing, add 0.5% stearic acid, temperature of reaction is 125 DEG C, terminate after oxygen flow 0.5L/ (hg wax), reaction 5h, sampling analysis, the results are shown in Table 1.
Table 1 stearic acid catalyzed oxidation result:
| Catalyst type | Acid number/(mgKOH/g) | Saponification value/(mgKOH/g) |
| Stearic acid | 28.19 | 57.11 |
Embodiment 2
Step, with example 1, will change boric acid into stearic acid, obtain final product, sampling analysis, the results are shown in Table 2.
Table 2 boric acid catalysis oxidation results:
| Catalyst type | Acid number/(mgKOH/g) | Saponification value/(mgKOH/g) |
| Boric acid | 28.5 | 61.02 |
Embodiment 3
Step, with example 1, changes stearic acid into tosic acid, obtains final product, and sampling analysis the results are shown in Table 3.
Table 3 Catalyzed by p-Toluenesulfonic Acid oxidation results
| Catalyst type | Acid number/(mgKOH/g) | Saponification value/(mgKOH/g) |
| Tosic acid | 27.86 | 62.87 |
Embodiment 4
40g coal wax is added in the there-necked flask of 500mL that thermometer, inlet pipe and offgas duct are housed, heat up fusing, add 0.5% stearic acid, temperature of reaction is 135 DEG C, oxygen flow 0.5L/ (hg wax), reaction 5h terminate, sampling analysis, the results are shown in Table 4.
Embodiment 5
Step, with example 4, changes temperature of reaction 125 DEG C into 150, obtains final product, sampling analysis, the results are shown in Table 4.
Embodiment 6
Step, with example 4, changes temperature of reaction 125 DEG C into 160 DEG C, obtains final product, sampling analysis, the results are shown in Table 4.
Embodiment 7
Step, with example 4, changes the reaction times into 3h by 5h, obtains final product, and sampling analysis the results are shown in Table 4.
Embodiment 8
Step, with example 4, changes the reaction times into 8h by 5h, obtains final product, and sampling analysis the results are shown in Table 4.
Embodiment 9
Step is with example 4, and change oxygen flow into 0.2L/ (hg wax) by 0.5L/ (hg wax), sampling analysis, the results are shown in Table 4.
Embodiment 10
Step is with example 4, and change oxygen flow 0.5L/ (hg wax) into 0.8L/ (hg wax), sampling analysis, the results are shown in Table 4.
The acid number of table 4 product, saponification value:
| Embodiment | Acid number/(mgKOH/g) | Saponification value/(mgKOH/g) |
| 4 | 27.86 | 62.87 |
| 5 | 28.01 | 63.04 |
| 6 | 28.81 | 65.8 |
| 7 | 27.89 | 59.30 |
| 8 | 27.50 | 59.00 |
| 9 | 27.37 | 51.09 |
| 10 | 28.46 | 66.15 |
The just the specific embodiment of the present invention described in above specification sheets, various illustrating is not construed as limiting flesh and blood of the present invention, person of an ordinary skill in the technical field after having read specification sheets can to before described embodiment make an amendment or be out of shape, and do not deviate from essence of an invention and scope.
Claims (3)
1. a technique for the waxed standby oxidized petroleum waves of matchmaker, is characterized in that: comprise the steps:
A () prepares raw material F-T coal wax, and add in there-necked flask, is warming up to 100 DEG C gradually and makes it melt;
B () adds the catalyzer that weight is 0.1% ~ 1.0% of F-T coal wax again;
C () passes into the oxygen of 0.2 ~ 0.8L/h according to each gram of F-T coal wax, this elementary reaction temperature controls at 125 DEG C ~ 160 DEG C, after reaction 3 ~ 8h, takes out product while hot and sampling analysis.
2. the technique of the waxed standby oxidized petroleum waves of a kind of matchmaker as claimed in claim 1, is characterized in that: described catalyzer is any in stearic acid, boric acid, tosic acid, or combinations several arbitrarily.
3. the technique of the waxed standby oxidized petroleum waves of a kind of matchmaker as claimed in claim 1, is characterized in that: the weight of described catalyzer is 0.5% of F-T coal wax.
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| CN201510582254.3A CN105087068B (en) | 2015-09-14 | 2015-09-14 | A kind of method of the waxed standby oxidized wax of coal |
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| CN201510582254.3A CN105087068B (en) | 2015-09-14 | 2015-09-14 | A kind of method of the waxed standby oxidized wax of coal |
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| CN105087068B CN105087068B (en) | 2018-01-30 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105733449A (en) * | 2016-03-18 | 2016-07-06 | 常州大学 | Process for preparing multifunctional vehicular emulsion by oxidized coal wax |
| CN112125990A (en) * | 2019-06-24 | 2020-12-25 | 内蒙古伊泰煤基新材料研究院有限公司 | Esterification modification method of wax |
| CN112852486A (en) * | 2021-01-12 | 2021-05-28 | 国家能源集团宁夏煤业有限责任公司 | Oxidized wax and preparation method thereof |
| CN113797867A (en) * | 2021-09-30 | 2021-12-17 | 内蒙古伊泰煤基新材料研究院有限公司 | Preparation method of continuous micro-channel of oxidized wax |
| CN115193363A (en) * | 2022-09-16 | 2022-10-18 | 世名(苏州)新材料研究院有限公司 | Oxidized wax with high acid value and low ester value, preparation process thereof and esterified wax prepared from oxidized wax |
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| US1947989A (en) * | 1928-06-20 | 1934-02-20 | Firm A Riebeck Sche Montanwerk | Method of oxidizing hydrocarbons |
| GB435385A (en) * | 1934-02-14 | 1935-09-16 | Ig Farbenindustrie Ag | Improvements in the manufacture and production of wetting, cleansing, dispersing andlike agents |
| GB902622A (en) * | 1958-07-23 | 1962-08-01 | British Petroleum Co | Improvements relating to the oxidation of residual petroleum waxes |
| CN1150216A (en) * | 1995-09-19 | 1997-05-21 | 本田技研工业株式会社 | Two-stroke IC engine |
| CN1150216C (en) * | 1998-07-30 | 2004-05-19 | 舒曼-萨索尔(南非)(控股)有限公司 | Waxes |
| CN101082000A (en) * | 2007-06-07 | 2007-12-05 | 上海焦耳蜡业有限公司 | Polyethylene wax polypropylene wax and petroleum wax co-oxidation method |
| CN104607115A (en) * | 2015-02-01 | 2015-05-13 | 南京天诗新材料科技有限公司 | Method and device for preparing oxidized wax |
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2015
- 2015-09-14 CN CN201510582254.3A patent/CN105087068B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US1947989A (en) * | 1928-06-20 | 1934-02-20 | Firm A Riebeck Sche Montanwerk | Method of oxidizing hydrocarbons |
| GB435385A (en) * | 1934-02-14 | 1935-09-16 | Ig Farbenindustrie Ag | Improvements in the manufacture and production of wetting, cleansing, dispersing andlike agents |
| GB902622A (en) * | 1958-07-23 | 1962-08-01 | British Petroleum Co | Improvements relating to the oxidation of residual petroleum waxes |
| CN1150216A (en) * | 1995-09-19 | 1997-05-21 | 本田技研工业株式会社 | Two-stroke IC engine |
| CN1150216C (en) * | 1998-07-30 | 2004-05-19 | 舒曼-萨索尔(南非)(控股)有限公司 | Waxes |
| CN101082000A (en) * | 2007-06-07 | 2007-12-05 | 上海焦耳蜡业有限公司 | Polyethylene wax polypropylene wax and petroleum wax co-oxidation method |
| CN104607115A (en) * | 2015-02-01 | 2015-05-13 | 南京天诗新材料科技有限公司 | Method and device for preparing oxidized wax |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105733449A (en) * | 2016-03-18 | 2016-07-06 | 常州大学 | Process for preparing multifunctional vehicular emulsion by oxidized coal wax |
| CN112125990A (en) * | 2019-06-24 | 2020-12-25 | 内蒙古伊泰煤基新材料研究院有限公司 | Esterification modification method of wax |
| CN112852486A (en) * | 2021-01-12 | 2021-05-28 | 国家能源集团宁夏煤业有限责任公司 | Oxidized wax and preparation method thereof |
| CN113797867A (en) * | 2021-09-30 | 2021-12-17 | 内蒙古伊泰煤基新材料研究院有限公司 | Preparation method of continuous micro-channel of oxidized wax |
| CN115193363A (en) * | 2022-09-16 | 2022-10-18 | 世名(苏州)新材料研究院有限公司 | Oxidized wax with high acid value and low ester value, preparation process thereof and esterified wax prepared from oxidized wax |
| CN115193363B (en) * | 2022-09-16 | 2023-02-24 | 世名(苏州)新材料研究院有限公司 | Oxidized wax with high acid value and low ester value, preparation process thereof and esterified wax prepared from oxidized wax |
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| CN105087068B (en) | 2018-01-30 |
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Inventor after: Xu Wengao Inventor after: Yang Jihe Inventor after: Gu Leilei Inventor after: Chen Ting Inventor after: Xu Ge Inventor after: Xu Xiaojiang Inventor before: Xu Wengao Inventor before: Yang Jihe Inventor before: Gu Leilei Inventor before: Chen Ting Inventor before: Xu Ge Inventor before: Xu Xiaohui |
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Granted publication date: 20180130 Termination date: 20180914 |