CN102977920B - Preparation method for food use microcrystalline waxes - Google Patents

Preparation method for food use microcrystalline waxes Download PDF

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CN102977920B
CN102977920B CN201210453636.2A CN201210453636A CN102977920B CN 102977920 B CN102977920 B CN 102977920B CN 201210453636 A CN201210453636 A CN 201210453636A CN 102977920 B CN102977920 B CN 102977920B
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microcrystalline wax
preparation
food
wax
hydrogen
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CN102977920A (en
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党渭铭
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Jiangxi Ruiqiyuan Technology Co ltd
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Wuxi Xinda Rosin & Ester System Co ltd
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Abstract

The invention provides a preparation method for food use microcrystalline waxes. The preparation method for the food use microcrystalline waxes includes that industrial microcrystalline waxes and catalysts are added into a hydrogenation reactor, and hydrogen is filled into the hydrogenation reactor, wherein hydrogen partial pressure is 10-15mPa, the volume ratio of the hydrogen to the waxes is 100-400, and the weight ratio of the catalysts to the waxes is 0.005-0.08; when the hydrogenation reactor is heated to be 75-85 DEG C, a stirrer of the hydrogenation reactor is started to stir; the hydrogenation reactor is heated continuously to be 280-300 DEG C for 1-2 hours, and then is cooled to be 240-260 DEG C for 2-3 hours; and materials are put in the hydrogenation reactor, the catalysts are filtered and removed, and the materials are cooled. The preparation method for the food use microcrystalline waxes is simple and convenient to operate, and saving in investment.

Description

The preparation method of Microcrystalline Wax for a kind of food
Technical field
The present invention relates to a kind of preparation method of Microcrystalline Wax, relate in particular to the preparation method of microcrystalline wax hydrogenation for a kind of food.
Background technology
Microcrystalline Wax is a kind of refining synthetic wax of approximate crystallite character, has good luster, and fusing point is high, the feature of lighter color, and its close structure, hard and lubricious, can melt mutually with various natural waxs, and can improve the fusing point of its low wax, improve the performance of thick property wax.The Microcrystalline Wax of most of grades has plasticity-.In color, Microcrystalline Wax is oyster white or faint yellow.In petroleum refining industry, Microcrystalline Wax is to separate from stay the residual oil still kettle by the solvent separation of series of complex.Microcrystalline Wax mainly by the naphthenic hydrocarbon of C30 1 and a small amount of just, isoparaffin forms, they have high-melting-point and unbodied feature.The fusing point of Microcrystalline Wax is generally 54.4OC 1 ' C, and paraffin, because it has the side chain hydro carbons of high-content, so have good snappiness, is difficult for broken relatively.Therefore, Microcrystalline Wax has application very widely in rubber plastic, automobile and other industries.It is also the material that medicine, makeup, food are deeply in love.
But industrial Microcrystalline Wax color is yellowish-brown, contains the objectionable impuritiess such as sulphur, nitrogen, condensed-nuclei aromatics, particularly condensed-nuclei aromatics has carinogenicity.International food, the general understanding of medical expert are that its hydrogenation is become to stable hydrocarbon, and human body is become to biologically inert material, harmless in health.CN1458244A discloses a kind of series hydrogenation refining process, at hydrogen dividing potential drop 10-16MPa, under the condition such as humidity 320-380 ℃, adopt fixed-bed reactor through secondary hydrogenation, catalyzer is a kind of or combination in transition metal W, Ni, Co, Mo, obtains and meets the Microcrystalline Wax of standard for FDA food.CN101240194A discloses a kind of two sections of medium-pressure hydrocracking technology and has compared with previous patent, has adopted hydrogen dividing potential drop 6-9mPa hydrogenation pressure, and fixed bed type reactor.The active metal component of catalyzer is a kind of or combination in W, Ni, Co, Mo, and hydrogenation is also met the Microcrystalline Wax of codex alimentarius.
Other similar patent, its type of reactor is fixed-bed type.Catalyzer is transition metal series.The difference such as temperature of reaction, pressure, bed array mode only.
This class technology is suitable for the large-tonnage industry application of large-lot producer.The deficiencies such as its investment is high, and device control requires high, and catalyzer is expensive, and the construction period is long.To fine chemicals, small but excellent production process, more difficult adaptation.
In view of this, how designing the preparation method of Microcrystalline Wax for a kind of food, with simple flow and cost-saving, is the problem that insider needs solution badly.
Summary of the invention
In prior art, while adopting fixed bed to prepare food use Microcrystalline Wax, the cycle is longer, and the more high defect of cost the invention provides a kind of preparation method of food use Microcrystalline Wax.
According to the present invention, the preparation method of a kind of food with Microcrystalline Wax is provided, wherein, comprising:
Industrial Microcrystalline Wax and catalyzer are added in hydriding reactor, pass into hydrogen, wherein, hydrogen dividing potential drop is 10~15mPa, and hydrogen wax volume ratio is 100~400, and catalyst wax weight ratio is 0.005~0.08, when being heated to 75~85 ℃, the agitator of described hydriding reactor starts to stir, and continues to be heated to 280~300 ℃ and continues 1~2h, is then cooled to 240~260 ℃ and continues 2~3h; And
Blowing, filters out described catalyzer, cooling.
Preferably, described catalyzer is for take the formate of transition metal as active metal component.
Preferably, described transition metal is a kind of in W, Ni, Co, Mo or their combination.
Preferably, by chuck, carry out electrically heated.
Preferably, described hydrogen dividing potential drop is 12~14mPa.
Preferably, described hydrogen wax volume ratio is 200~300.
Preferably, described catalyst wax weight ratio is 0.02~0.05.
Preferably, described agitator is turbine type, push type or hinged joint oar formula.
Preferably, the rotating speed of described agitator is 100~250 revs/min.
Advantage of the present invention is: by hydriding reactor, industrial Microcrystalline Wax being carried out to hydrogenation reaction, hydrogenation reaction is divided into two stages: in relatively-high temperature stage first stage, hydrogenation carries out denitrogenation, desulfurization, deoxidation to industrial Microcrystalline Wax; In the second relative low temperature stage, hydrogenation carries out aromatic saturation reaction, and this process is easier, the suitable preparation Microcrystalline Wax in a small amount that is used for, and catalyzer wherein can recycle, has reduced cost.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, to the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skills, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 shows the structural representation according to hydriding reactor of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Fig. 1 shows the structural representation according to hydriding reactor of the present invention.With reference to Fig. 1, hydriding reactor comprises: kettle 10, on kettle 10, be provided with entrance 101 and inlet mouth 102, and be also provided with the agitator 11 stretching in kettle 10, agitator 11 can be turbine type, push type or hinged joint oar formula.Can add industrial Microcrystalline Wax and catalyzer from entrance 101 phase kettlies 10, from inlet mouth 102, pass into hydrogen, 11, agitator stirs in heat-processed, and the rotating speed of agitator 11 is 100~250 revs/min.
Embodiment 1
In 1L medium-pressure hydrocracking still, add industrial Microcrystalline Wax 400g and catalyzer nickel formate 2g, pass into hydrogen, wherein, hydrogen dividing potential drop is 10mPa, hydrogen wax volume ratio is 100.While being then heated to 75 ℃ by chuck, agitator starts to stir with 100 revs/min of rotating speeds, continues to be heated to 280 ℃, and 1h is to carry out desulfurization, denitrogenation, deoxygenation in reaction.Next, be cooled to 240 ℃, 2h is to carry out aromatic saturation reaction in reaction.Finally, material is from hydriding reactor flows out, and through gas-liquid separation and filter out after catalyzer nickel formate, color is reduced to 2 (GB/T-6540) from look numbers 5, obviously white by xanthochromia, then the cooling Microcrystalline Wax that obtains.
Embodiment 2
In 1L medium-pressure hydrocracking still, add industrial Microcrystalline Wax 400g and catalyzer formic acid tungsten 8g, pass into hydrogen, wherein, hydrogen dividing potential drop is 11mPa, hydrogen wax volume ratio is 200.While being then heated to 80 ℃ by chuck, agitator starts to stir with 130 revs/min of rotating speeds, continues to be heated to 290 ℃, and 1.5h is to carry out desulfurization, denitrogenation, deoxygenation in reaction.Next, be cooled to 250 ℃, 2.5h is to carry out aromatic saturation reaction in reaction.Finally, material is from hydriding reactor flows out, and through gas-liquid separation and filter out after catalyzer nickel formate, Ghana's look number is reduced to 2 (GB/T-6540) from 5, obviously white by xanthochromia, then the cooling Microcrystalline Wax that obtains.
Embodiment 3
In 1L medium-pressure hydrocracking still, add industrial Microcrystalline Wax 400g and catalyzer formic acid molybdenum 14g, pass into hydrogen, wherein, hydrogen dividing potential drop is 12mPa, hydrogen wax volume ratio is 300.While being then heated to 85 ℃ by chuck, agitator starts to stir with 160 revs/min of rotating speeds, continues to be heated to 300 ℃, and 2h is to carry out desulfurization, denitrogenation, deoxygenation in reaction.Next, be cooled to 260 ℃, 3h is to carry out aromatic saturation reaction in reaction.Finally, material is from hydriding reactor flows out, through gas-liquid separation and filter out after catalyzer nickel formate, Ghana's look number is reduced to < 1 (GB/T-6540) from 4.5, then the cooling Microcrystalline Wax that obtains, during uv-absorbing light 280~289nm, from 1.2, reducing to 0.14(codex alimentarius is 0.15) meet food grade requirement.
Embodiment 4
In 1L medium-pressure hydrocracking still, add industrial Microcrystalline Wax 400g and catalyzer formic acid tungsten 16g, pass into hydrogen, wherein, hydrogen dividing potential drop is 13mPa, hydrogen wax volume ratio is 400.While being then heated to 80 ℃ by chuck, agitator starts to stir with 190 revs/min of rotating speeds, continues to be heated to 295 ℃, and 1.5h is to carry out desulfurization, denitrogenation, deoxygenation in reaction.Next, be cooled to 245 ℃, 2.5h is to carry out aromatic saturation reaction in reaction.Finally, material is from hydriding reactor flows out, and through gas-liquid separation and filter out after catalyzer nickel formate, Ghana's look number is reduced to 2 (GB/T-6540) from 5, obviously white by xanthochromia, then the cooling Microcrystalline Wax that obtains.
Embodiment 5
In 1L medium-pressure hydrocracking still, add industrial Microcrystalline Wax 400g and catalyzer nickel formate 20g, pass into hydrogen, wherein, hydrogen dividing potential drop is 14mPa, hydrogen wax volume ratio is 150.While being then heated to 80 ℃ by chuck, agitator starts to stir with 250 revs/min of rotating speeds, continues to be heated to 285 ℃, and 1.3h is to carry out desulfurization, denitrogenation, deoxygenation in reaction.Next, be cooled to 255 ℃, 2.5h is to carry out aromatic saturation reaction in reaction.Finally, material is from hydriding reactor flows out, and through gas-liquid separation and filter out after catalyzer nickel formate, Ghana's look number is reduced to 2 (GB/T-6540) from 5, obviously white by xanthochromia, then the cooling Microcrystalline Wax that obtains.
Embodiment 6
In 1L medium-pressure hydrocracking still, add industrial Microcrystalline Wax 400g and catalyzer nickel formate 32g, pass into hydrogen, wherein, hydrogen dividing potential drop is 15mPa, hydrogen wax volume ratio is 350.While being then heated to 80 ℃ by chuck, agitator starts to stir with 175 revs/min of rotating speeds, continues to be heated to 295 ℃, and 1.3h is to carry out desulfurization, denitrogenation, deoxygenation in reaction.Next, be cooled to 260 ℃, 2.5h is to carry out aromatic saturation reaction in reaction.Finally, material is from hydriding reactor flows out, and through gas-liquid separation and filter out after catalyzer nickel formate, Ghana's look number is reduced to 2 (GB/T-6540) from 5, obviously white by xanthochromia, then the cooling Microcrystalline Wax that obtains.
Advantage of the present invention is: by hydriding reactor, industrial Microcrystalline Wax being carried out to hydrogenation reaction, hydrogenation reaction is divided into two stages: in relatively-high temperature stage first stage, hydrogenation carries out denitrogenation, desulfurization, deoxidation to industrial Microcrystalline Wax; In the second relative low temperature stage, hydrogenation carries out aromatic saturation reaction, and this process is easier, the suitable preparation Microcrystalline Wax in a small amount that is used for, and catalyzer wherein can recycle, has reduced cost.
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.

Claims (8)

1. a preparation method for Microcrystalline Wax for food, is characterized in that, comprising:
Industrial Microcrystalline Wax and catalyzer are added in hydriding reactor, pass into hydrogen, wherein, hydrogen dividing potential drop is 10~15mPa, and hydrogen wax volume ratio is 100~400, catalyzer is for take the formate of transition metal as active metal component, catalyst wax weight ratio is 0.005~0.08, and when being heated to 75~85 ℃, the agitator of hydriding reactor starts to stir, continue to be heated to 280~300 ℃ and continue 1~2h, be then cooled to 240~260 ℃ and continue 2~3h; Blowing, filters out catalyzer, cooling.
2. the preparation method of Microcrystalline Wax for a kind of food as claimed in claim 1, is characterized in that, described transition metal is a kind of in W, Ni, Co, Mo or their combination.
3. the preparation method of Microcrystalline Wax for a kind of food as claimed in claim 1, is characterized in that, described hydriding reactor carries out electrically heated by chuck.
4. the preparation method of Microcrystalline Wax for a kind of food as described in claims 1 to 3 any one claim, is characterized in that, described hydrogen dividing potential drop is 12~14mPa.
5. the preparation method of Microcrystalline Wax for a kind of food as described in claims 1 to 3 any one claim, is characterized in that, described hydrogen wax volume ratio is 200~300.
6. a kind of preparation method of food use Microcrystalline Wax as described in claims 1 to 3 any one claim, is characterized in that, described catalyst wax weight ratio is 0.02~0.05.
7. the preparation method of Microcrystalline Wax for a kind of food as described in claims 1 to 3 any one claim, is characterized in that, described agitator is turbine type, push type or hinged joint oar formula.
8. the preparation method of Microcrystalline Wax for a kind of food as described in claims 1 to 3 any one claim, is characterized in that, the rotating speed of described agitator is 100~250 revs/min.
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CN104650979A (en) * 2013-11-21 2015-05-27 无锡信达胶脂材料股份有限公司 Kettle type hydrogenation method for paraffin or microcrystalline wax
CN105602620B (en) * 2015-11-17 2017-11-07 吕志超 A kind of preparation method of food-grade paraffin wax
CN107321294A (en) * 2017-08-03 2017-11-07 荆门市双创专利技术服务有限公司 A kind of production line of edible vaseline
CN108031462A (en) * 2017-12-05 2018-05-15 广州高八二塑料有限公司 It is used to prepare the catalyst of food-grade paraffin wax and the preparation method of food-grade paraffin wax
CN109988637B (en) * 2017-12-29 2021-05-04 中国石油化工股份有限公司 Flexible paraffin hydrogenation process

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