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Preparation method of food-grade microcrystalline wax

A microcrystalline wax, food-grade technology, applied in the field of petroleum microcrystalline wax preparation, can solve the problems of narrow selection range of raw material wax, large material loss, high quality requirements, etc., to reduce production links and environmental pollution, improve selectivity, The effect of increasing severity

Inactive Publication Date: 2014-06-18
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process of the first three food-grade microcrystalline waxes is to firstly process paraffin-based deasphalted oil through solvent refining and solvent dewaxing to obtain deoiled microcrystalline wax, and then according to the properties of the crude microcrystalline wax, undergo hydrogenation treatment and aromatic hydrocarbon addition. Hydrogen saturation is used to prepare the target product microcrystalline wax. The main defects of this type of process route are: (1) The process route is long, energy consumption is high, material loss in the production process is large, and product yield is low
(2) Limited by the preparation process, the selection range of raw material wax is narrow
[0006] It can be seen from the above-mentioned disclosed technical schemes of documents that the existing food-grade microcrystalline wax product preparation process is mainly to firstly prepare coarse microcrystalline wax, and then use it as a raw material to obtain a food-grade microcrystalline wax product through a hydrogenation process using a suitable catalyst. , this route mainly has defects such as narrow selection of raw material wax, high quality requirements, and special catalyst performance requirements.

Method used

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  • Preparation method of food-grade microcrystalline wax
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  • Preparation method of food-grade microcrystalline wax

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Paraffin-based deasphalted oil and naphthenic deasphalted oil were fully mixed at a weight percentage of 96:4. The properties of paraffin-based deasphalted oil, naphthenic deasphalted oil, and blended oil A after mixing are shown in Table 1.

[0022] The mixed oil enters the two-stage hydrogenation reactor for hydrogenation reaction, and the hydrogenated oil obtained is fractionated and cut to obtain a heavy fraction at 480°C to 750°C. The operating parameters of the reaction conditions and the property analysis of the heavy fraction are shown in Table 2. Catalyst property analysis See the first set of catalyst systems in Table 4.

[0023] 480℃~750℃ heavy distillate, mixed with dewaxing solvent at a ratio of 1:4, the dewaxing solvent is a mixture of butanone and toluene, in which the weight of butanone accounts for 50% of the mixture, and toluene accounts for 50%, gradually cool down to lower the temperature To -20°C, after filtration, wax filtrate and oily wax paste ar...

Embodiment 2

[0025] Using the blended oil A raw material and hydrogenation process conditions in implementation 1, the hydrogenation catalyst is selected as the second group of catalysts in Table 4, and the heavy fraction at 480°C to 750°C is mixed with the dewaxing solvent, and the dewaxing solvent is acetone and benzene The mixture, wherein the weight of acetone accounts for 70% of the mixture, benzene accounts for 30%, gradually cooled down to -15 ° C, filtered to obtain wax filtrate and oil-containing wax paste, after recovery of oil-containing wax paste, deoiled wax is obtained, and the obtained de-oiled wax is obtained. Oily wax is mixed with 5% (mass fraction) clay, and described clay is commercially available clay, stirred at 130 DEG C for 10 minutes, filtered to obtain food-grade microcrystalline wax product after removing clay, and the yield of food-grade microcrystalline wax product and The property analysis is shown in Table 5.

Embodiment 3

[0027] Using the blended oil A raw material and hydrogenation process conditions in implementation 1, the hydrogenation catalyst is selected as the third group of catalysts in Table 4, and the heavy fraction at 480°C to 750°C is mixed with the dewaxing solvent, and the dewaxing solvent is methyl ethyl ketone and A mixture of benzene, wherein the weight of butanone accounts for 70% of the mixture, and benzene accounts for 30%. Gradually cool down and lower the temperature to -15°C. After filtration, wax filtrate and oily wax paste are obtained. After the oily wax paste is recovered, deoiled wax is obtained. The deoiled wax is mixed with 10% (mass fraction) of white clay, the white clay is commercially available white clay, stirred at 110°C for 20 minutes, and the food-grade microcrystalline wax product is obtained after filtering and removing the white clay, and the food-grade microcrystalline wax product is collected See Table 5 for rate and property analysis.

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Abstract

The invention relates to a preparation method of food-grade microcrystalline wax. The preparation method comprises the following steps that blended oil comprising paraffin-based slag-reduced deasphalted oil and naphthenic base slag-reduced deasphalted oil is used as a raw material, is fed into a first reaction bed layer and then undergoes a hydrotreatment modification reaction; the reaction product is fed into a stripping tower and the stripped product is fed into a second reaction bed layer and undergoes a hydrofining reaction to produce hydrofined product oil; the hydrofined product oil is cut by atmospheric and vacuum fractionation equipment to form a heavy lubricant component having a temperature of 480-750 DEG C; the heavy lubricant component and an acetone-benzol dewaxing solvent are mixed; the mixture is cooled to below -15 DEG C; the cooled mixture is filtered so that dewaxed filtrate and deoiled wax are obtained; the deoiled wax is mixed with carclazyte by stirring; and the mixture is filtered so that the carclazyte is removed and the food-grade microcrystalline wax is obtained. The food-grade microcrystalline wax has Seybolt color number greater than +25, a drop melting point of 67-92 DEG C, a needle penetration degree of 15-35(1 / 10mm), oil content of 0.85-3.0%, sulfur and nitrogen content less than 1 microgram per gram and heavy metal and arsenic content less than 1mg / kg.

Description

technical field [0001] The invention relates to a preparation method of petroleum wax, in particular to a preparation method of petroleum microcrystalline wax. Background technique [0002] Microcrystalline wax is an important raw material for medicine, daily chemical industry and other fine chemical products. Microcrystalline wax is the degassed wax obtained when lubricating oil is refined from the vacuum residue produced by atmospheric and vacuum equipment. Its main components are cyclic hydrocarbons with normal or isomeric alkyl side chains, especially naphthenes. Refined microcrystalline wax, that is, crude crystalline wax, contains more sulfur, nitrogen, oxygen heteroatom compounds and aromatic compounds, and also contains a small amount of polymer condensed ring compounds such as colloidal asphaltenes. [0003] According to the existing production process, microcrystalline wax is a product processed by solvent deasphalting, solvent refining, solvent dewaxing and deoil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10G73/44
Inventor 汪军平王华田凌燕甄新平熊春珠魏军朱路新
Owner PETROCHINA CO LTD
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