CN105087068B - A kind of method of the waxed standby oxidized wax of coal - Google Patents
A kind of method of the waxed standby oxidized wax of coal Download PDFInfo
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- CN105087068B CN105087068B CN201510582254.3A CN201510582254A CN105087068B CN 105087068 B CN105087068 B CN 105087068B CN 201510582254 A CN201510582254 A CN 201510582254A CN 105087068 B CN105087068 B CN 105087068B
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Abstract
The present invention relates to a kind of technique of the waxed standby oxidized wax of coal, comprise the following steps：Prepare raw material F T coal waxes, and add in three-necked flask, be gradually heating to 100 DEG C and make its fusing；Add 0.1%~1.0% catalyst that weight is F T coal waxes；0.2~0.8L/h oxygen is passed through according to each gram of F T coal waxes, this elementary reaction temperature control is at 125 DEG C~160 DEG C, after reacting 3~8h, takes out product and sampling analysis while hot.The present invention substitutes prior paraffin with F T coals wax and prepares oxidized wax, alleviates the pressure of petroleum resources shortage, improves the economic value added of coal wax；The materials such as heavy metal ion catalyst, nitrogen protection gas, water entrainer and reagent and additive in polymerization are not used；Reaction time is short, easy to operate, and the oxidized wax product color of preparation is shallow, and smell is light, and acid number, saponification number reach South Africa SASOLWAX A28 index requests；The technique does not need special process equipment.
Description
Technical field
The present invention relates to the preparation field of oxidized wax, the method for the waxed standby oxidized wax of especially a kind of coal.
Background technology
Wax has extensive purposes in rubber and plastic industry, coating, ink area and daily chemical industry.Wax passes through different degrees of
Oxidation modification, taken on its long linear hydroxyl, carboxyl, ester group and be provided with certain polarity, with fluoropolymer resin, have
Machine inorganic color stuffing has more preferable compatibility, can be emulsified in water, so as to expand the application of wax.
Wax can include paraffin, microwax, Fischer-Tropsch wax, Tissuemat E, polypropylene wax etc..The index of the degree of oxidation of wax
It can be the acid number of the oxidation product of wax, that is, neutralize the KOH milligram numbers needed for 1 gram of (g) sample, represented with mgKOH/g.Oxidized wax
It generally may be used as brightener of the inside and outside lubricant agent of PVC processing, the Ricinate of filling master batch and color masterbatch, rubber etc.
Deng can be used for preparing wax emulsion and daily chemical products, saponification, esterified wax can also be further processed into.
CN104178219A discloses a kind of method of F- T synthesis waxy stone production microwax, wherein disclosing：With generation
The increasingly exhausted and continuous enhancing to environmental protection consciousness of boundary's petroleum resources, research is with finding environment-friendly petroleum-based energy
Substitute turns into one of direction of world-technology exploitation.Pass through F- T synthesis (Fischer- with coal and natural gas
TropschSynthesis) reaction prepares coal wax and replaces prior paraffin, on the one hand can solve petroleum resources shortage problem, full
Demand of the sufficient national economy rapid growth to the energy；On the other hand the economic value added of Fischer-Tropsch wax can be improved, while can be with
Environmental pollution caused by directly burning is reduced, it is significant.
Document [development and application that paraffin oxidation is modified, Liaoning chemical industry, 2009,38 (9)：670~673] disclose：Closely
Nian Lai, although China makes some progress in terms of oxidized wax is developed, there is some following deficiency：Do not formed large-scale
Exploitation, produce and using situation；Oxidized wax color is deep, smell is heavy, second-rate；The indexs such as acid number, saponification number, which can not meet, to be needed
Ask, limit its use；The impurity such as the catalyst containing remaining and the friendship matter of reaction generation.
CN103468316A discloses a kind of preparation method of peracid soap oxidized wax, disclose using manganese salt (manganese sulfate) as
The method of catalyst preparation oxidized wax, although the product acid number reaches 23.71mgKOH/g, saponification number reaches 49.13mgKOH/g,
In oxygen atmosphere, metal ion can be oxidized production metal oxide and other accessory substances, deepen coloured product, reduce catalyst
Activity.
CN1206719A discloses a kind of by oxygen or oxygenous admixture of gas melt oxidation is by metallocene catalyst
Alathon and the method for copolymer waxes prepared by agent, the acid number 18.00mgKOH/g of its oxidized wax prepared, saponification number
40mgKOH/g。
[development of hardening oxidation wax, petrochemical technology is with applying .2007,25 (4) for document：314~315] a kind of nitrogen has been reported
The method that hardening oxidation wax is produced under the conditions of gas shielded；
CN101289540A, CN101724107A disclose Tissuemat E or the method for oxidation of ethene wax emulsion.
From above-mentioned disclosed patent and document, F-T waxes synthesis microwax, paraffin oxidation, Tissuemat E oxygen are related to
The report of change, but the report of also no F-T coals wax oxidation, its correlative study direction value obtain further investigated both at home and abroad so far.
The content of the invention
The technical problem to be solved in the present invention is：It is proposed that substituting prior paraffin with F-T coals wax prepares the new of oxidized wax
Technique.
The technical solution adopted in the present invention is：A kind of technique of the waxed standby oxidized wax of matchmaker, comprises the following steps：
(a) prepare raw material F-T coal waxes, and add in three-necked flask, be gradually heating to 100 DEG C and make its fusing；
(b) 0.1%~1.0% catalyst that weight is F-T coal waxes is added；
(c) 0.2~0.8L/h oxygen is passed through according to each gram of F-T coal waxes, this elementary reaction temperature control is at 125 DEG C
~160 DEG C, after reacting 3~8h, product and sampling analysis are taken out while hot.
Further, it is stearic acid, boric acid, to first as a kind of specific embodiment, heretofore described catalyst
It is any in benzene sulfonic acid, or any several combination.
Further, as a kind of specific embodiment, the weight of heretofore described catalyst is F-T coal waxes
0.5%
The beneficial effects of the invention are as follows：Mainly have it is following some：
(1) prior paraffin is substituted with F-T coals wax and prepares oxidized wax, alleviate the pressure of petroleum resources shortage, improve coal system
The economic value added of wax；
(2) technique does not use the materials such as heavy metal ion catalyst, nitrogen protection gas, water entrainer and reagent and additive in polymerization；
(3) the technological reaction time is short, easy to operate, and the oxidized wax product color of preparation is shallow, and smell is light, acid number, saponification
Value reaches South Africa SASOLWAXA28 index requests；
(4) technique does not need special process equipment.
Embodiment
Presently in connection with preferred embodiment, the present invention is further detailed explanation.
Embodiment 1
40g coal waxes are added in the three-necked flask of the 500mL equipped with thermometer, air inlet pipe and offgas duct, heating is melted,
Add 0.5% stearic acid, reaction temperature is] 25 DEG C, oxygen flow 0.5L/ (hg waxes), terminate after reaction 5h, sampling analysis,
It the results are shown in Table 1.
The stearic acid catalysis oxidation result of table 1：
| Catalyst type | Acid number/(mgKOH/g) | Saponification number/(mgKOH/g) |
| Stearic acid | 28.19 | 57.11 |
Embodiment 2
Step will be changed to boric acid to stearic acid, and obtain final product, sampling analysis, the results are shown in Table 2 with example 1.
The boric acid catalysis oxidation results of table 2：
| Catalyst type | Acid number/(mgKOH/g) | Saponification number/(mgKOH/g) |
| Boric acid | 28.5 | 61.02 |
Embodiment 3
Stearic acid is changed to p-methyl benzenesulfonic acid, obtains final product, sampling analysis, the results are shown in Table 3 by step with example 1.
The Catalyzed by p-Toluenesulfonic Acid oxidation results of table 3
| Catalyst type | Acid number/(mgKOH/g) | Saponification number/(mgKOH/g) |
| P-methyl benzenesulfonic acid | 27.86 | 62.87 |
Embodiment 4
40g coal waxes are added in the three-necked flask of the 500mL equipped with thermometer, air inlet pipe and offgas duct, heating is melted,
Add 0.5% stearic acid, reaction temperature is 135 DEG C, oxygen flow 0.5L/ (hg waxes), reaction 5h terminate, sampling analysis, knot
Fruit is shown in Table 4.
Embodiment 5
For step with example 4, by reaction temperature, 125 DEG C are changed to 150, obtain final product, sampling analysis, the results are shown in Table 4.
Embodiment 6
For step with example 4, by reaction temperature, 125 DEG C are changed to 160 DEG C, obtain final product, sampling analysis, the results are shown in Table 4.
Embodiment 7
Reaction time is changed to 3h by 5h, obtains final product, sampling analysis, the results are shown in Table 4 by step with example 4.
Embodiment 8
Reaction time is changed to 8h by 5h, obtains final product, sampling analysis, the results are shown in Table 4 by step with example 4.
Embodiment 9
Step is changed to 0.2L/ (hg waxes) with example 4, by oxygen flow by 0.5L/ (hg waxes), sampling analysis, as a result
It is shown in Table 4.
Embodiment 10
Oxygen flow 0.5L/ (hg waxes) is changed to 0.8L/ (hg waxes), sampling analysis, as a result seen by step with example 4
Table 4.
The acid number of the product of table 4, saponification number：
| Embodiment | Acid number/(mgKOH/g) | Saponification number/(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 embodiment of the simply present invention described in description above, various illustrations are not to the reality of the present invention
Matter Composition of contents limits, and person of an ordinary skill in the technical field can be to described in the past specific after specification has been read
Embodiment is made an amendment or deformed, without departing from the spirit and scope of invention.
Claims (2)
- A kind of 1. technique of the waxed standby oxidized wax of matchmaker, it is characterised in that：Comprise the following steps：(a) prepare raw material F-T coal waxes, and add in three-necked flask, be gradually heating to 100 DEG C and make its fusing；(b) 0.1%~1.0% catalyst that weight is F-T coal waxes is added；(c) be passed through 0.2~0.8L/h oxygen according to each gram of F-T coal waxes, this elementary reaction temperature control 125 DEG C~ 160 DEG C, after reacting 3~8h, product and sampling analysis are taken out while hot,The catalyst is stearic acid, any in boric acid, p-methyl benzenesulfonic acid, or any several combination.
- A kind of 2. technique of the waxed standby oxidized wax of matchmaker as claimed in claim 1, it is characterised in that：The weight of the catalyst is The 0.5% of F-T coal waxes.
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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 true CN105087068B (en) | 2018-01-30 |
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Families Citing this family (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 |
| CN112852486B (en) * | 2021-01-12 | 2022-10-14 | 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 |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1947989A (en) * | 1928-06-20 | 1934-02-20 | Firm A Riebeck Sche Montanwerk | Method of oxidizing hydrocarbons |
| 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 |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| AU704849B2 (en) * | 1995-09-19 | 1999-05-06 | Honda Giken Kogyo Kabushiki Kaisha | Two-cycle internal combustion engine |
| JP2002521536A (en) * | 1998-07-30 | 2002-07-16 | シューマン サソル （サウス アフリカ）（プロプライエタリイ）リミテッド | wax |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1947989A (en) * | 1928-06-20 | 1934-02-20 | Firm A Riebeck Sche Montanwerk | Method of oxidizing hydrocarbons |
| 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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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 |