CN1022180C - Process for preparing solid decolorizer - Google Patents

Process for preparing solid decolorizer Download PDF

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Publication number
CN1022180C
CN1022180C CN 90104205 CN90104205A CN1022180C CN 1022180 C CN1022180 C CN 1022180C CN 90104205 CN90104205 CN 90104205 CN 90104205 A CN90104205 A CN 90104205A CN 1022180 C CN1022180 C CN 1022180C
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CN
China
Prior art keywords
saccharification
temperature
described method
charing
vitriol oil
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Expired - Fee Related
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CN 90104205
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Chinese (zh)
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CN1054754A (en
Inventor
张建洲
时运铭
杨秀芬
何锦凯
李成显
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INST OF PETRO-CHEMICAL INDUSTRY HEBEI PROV
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INST OF PETRO-CHEMICAL INDUSTRY HEBEI PROV
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Priority to CN 90104205 priority Critical patent/CN1022180C/en
Publication of CN1054754A publication Critical patent/CN1054754A/en
Application granted granted Critical
Publication of CN1022180C publication Critical patent/CN1022180C/en
Anticipated expiration legal-status Critical
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Abstract

The present invention relates to a preparation method of a solid decolorizer. A dry and pulverized plant fiber material is taken to be mixed with concentrated sulfuric acid in a ratio of 1: 1 to 4, and the reaction temperature is controlled in a range of 10 to 100 DEG C. Firstly, the material is saccharified, and then, the saccharifying liquid is carbonized at 150 to 280 DEG C. high temperature. Afterward, the solid decolorizer is obtained through workinging procedures of washing, fine grinding, etc.

Description

Process for preparing solid decolorizer
The present invention relates to a kind of preparation method of solid decolorizer.
The discoloring agent that extensively adopts at industrial sectors such as food-processing, light industry, environmental protection, pharmacy, chemical industry is a gac.Because gac has characteristics such as hole is many, specific surface area is big, and adsorption activity is strong, be the sorbent material or the discoloring agent of people's first-selection therefore, and the consumption of gac is also very big in industrial application always.
It is the Woody plant raw material that the industrial raw material that is used to prepare gac adopts maximum, as wood chip, lignin, branch, charcoal, shell etc., what production method was commonly used is the chemical agent activation method, and this method is raw material to be added auxiliary reagent mix and stir after screening, drying, carries out operations such as charing, recovery, rinsing again, the auxiliary reagent that is added is many, complex process, reaction yield is low, the product cost height, and have pollution problem, particularly need to consume a large amount of useful timber.However, because the needs of producing, this method people use till today always.Therefore, seek new gac surrogate,, significance is arranged to improve decolorizing efficiency and to reduce product cost.
The preparation method who the purpose of this invention is to provide a kind of solid decolorizer extensive, that technology is simple, cost is low, decolorizing effect is high of drawing materials.
The object of the present invention is achieved like this.Get drying, comminuted plants fibre material in container with normal temperature under the vitriol oil mix with certain proportion, control reaction temperature within the specific limits, at first make the material saccharification, then with the charing in the limiting time at high temperature of saccharification liquid, obtain a kind of solid decolorizer through washing, operation such as levigate again.
Feature of the present invention comprises:
(a) with drying after comminuted plants fibre material and the vitriol oil with 1: the weight ratio of 1-4 is mixed, and control reaction temperature 10-100 ℃, makes the material saccharification;
(b) saccharification liquid carries out charing under temperature 150-230 ℃ that limits and limiting time 10-100 minute condition,
(c) material of charing washes with water
Feature of the present invention also comprises:
Required raw material is plant material or the plant material of cellulose or their mixture that contains xylogen, straw, root or shell, wood chip etc. as farm crop, the material mass dryness fraction is that water content is 5-10%, be crushed to granularity 0.1-20 millimeter scope all can, used vitriol oil concentration can be selected in the 80-98% scope.
10-100 ℃ of saccharification react controlled temperature, feed way can adopt the vitriol oil to add in the material; Also can adopt material to be added in the vitriol oil; Perhaps adopt the limit to add the hybrid mode that vitriol oil limit adds material.By the control feed rate can control reaction temperature at limited range.
Saccharification react and carbonization process divide two steps to carry out, and are preferably in the different containers and carry out, and can control reaction conditions well like this, help operation.
The mixed weight ratio of material and the vitriol oil is preferably 1: 2.0-3.5.
Control reaction temperature is preferably in 40-70 ℃ during saccharification.
The material that saccharification is good carries out high temperature carbonization and is preferably in 170-230 ℃, and limiting time 25-55 minute more suitable.
The material that charing is good washs with tap water, and with the unnecessary sulfuric acid of flush away, the consumption of washing water is 3-12 a times of charing liquid weight of material, generally is controlled at 5-10 and doubly gets final product, and washing water can once or several times add.
The material that washing is good can levigate as required and packing after dehydration.
Adopt the solid decolorizer of method preparation of the present invention, see as coke shape particulate from profile, through evidence, it is not simple charcoal, because of it has molecular adsorption and two kinds of performances of ion-exchange concurrently, but also have the character of nitrogenous substances colloid and part calcium salt in the adsorption treatment liquid, thus its in application than the quality that more can improve processed liquid with gac, therefore, can replace gac to a certain extent.
It may be noted that gac divides multiple model as discoloring agent, to be suitable for different purposes, but can not use alternately, activated carbon decolorizing generally needs just can demonstrate good effect with heat decoloring, and bleaching temperature is between 70-100 ℃, and promptly destainer need be heated to the necessary requirement temperature.Discoloring agent of the present invention is through evidence, and to not had particular requirement by destainer, temperature can be received good effect in 10-100 ℃.With regard to discoloring agent of the present invention, there is no the difference of model simultaneously, then very convenient when therefore using.
Solid decolorizer end properties of the present invention is stable.Deposit in order to investigate, transportation, packaging Problems, once did such work, having carried out 54,35,20,2 ,-4 ,-8 ,-18 ℃ of temperature storage period stores, got the same in per 5 days in storage period, carry out Decolorant Test, stored the result in one month and show when depositing for 35--18 ℃, percent of decolourization almost not to be had influence, deposit a month percent of decolourization for 54 ℃ and reduce<10%.Also did following work: carry out continuous 24 hours vibration experiments in bobbing machine, solid-liquid separation does not appear in product.It seems that its water content is stable, the product after the vibration does not have influence to percent of decolourization.
Method characteristics of the present invention are that reacting balance, processing ease, reaction time are short.Elder generation's saccharification can make the raw molecule amount greatly reduce, and active group increases.Because temperature of reaction is low, adds sour safety, control easily, the container material solves easily, is fit to large-scale industrial production.
Method raw material sources of the present invention are extensive, reduced facility investment, save energy, throughput is big, is a kind of novel method that develops agricultural byproducts, also is the new way of an alternative activated carbon decolorizing.
Can further specify by the following specific embodiments and the objective of the invention is how to realize.
Embodiment 1:
Take by weighing through super-dry, granularity corn stalk 500 grams, take by weighing 92.5% sulfuric acid 1500 grams less than 10 millimeters.The vitriol oil is added in 2000 ml beakers of band stirring and thermometer earlier, start stirring, slowly add corn stalk, corn stalk adds speed so that saccharification temperature remains on 40 ± 2 ℃.After material adds, fully stir, so that saccharification react is complete.
The material that saccharification is good is moved into oil bath and is heated in 230 ℃ the asher, and asher is equipped with and stirs and thermometer, and under agitation, material kept 30 minutes in 220 ℃.After the cooling, obtain charing material 1350 grams.Approximately wash at twice immediately with 12150 gram tap water, through dehydration, ball milling, pack product 350 gram.
Embodiment 2:
Take by weighing through super-dry, granularity wood chip 2000 grams less than 5 millimeters, get earlier 1/3 of total amount join have stir and the saccharification react device of thermometer in.Start stirring, slowly add 95% sulfuric acid totally 5000 grams, simultaneously,, remaining wood chip is also slowly joined in the saccharification react device along with vitriolic adds.Feed rate is so that the saccharification react temperature is no more than 70 ± 2 ℃ is advisable.After two kinds of materials add, fully stir, so that saccharification react is complete.
The material that saccharification is good moves in the enamel tray, puts into the charing case that is heated to 200 ℃ in advance and carries out charing.Carbonization temperature kept 50 minutes at 200 ℃, after the cooling, got charing material 5000 grams.Restraining from the beginning with 25000 then, moisture washs for 4 times.The material that washing is good restrains through dewatering, grind, pack, get product 1440.
Embodiment 3:
Take by weighing through pulverizing, amalgamation material that granularity is crossed less than 20 millimeters and drying totally 4000 grams, wheat straw 1000 grams wherein, paddy stalk 1000 grams, wood chip 1000 grams, sugarcane slag 1000 grams.Splicing object is joined in the saccharification react device that stirring and thermometer are housed, start stirring, slowly add 98% sulfuric acid 8000 grams, sulfuric acid adds speed so that saccharification react remains on 55 ± 2 ℃ is advisable, after adding sulfuric acid, fully stir, so that saccharification react carries out fully.
The material that saccharification is good moves in the enamel tray, puts into the charing case that is heated to 190 ℃ in advance, and carbonization time kept 35 minutes.After the cooling, get charing material 11800 grams, divide secondary washing with 94400 ml tap waters then.Washing material well gets product 2920 grams through dehydration, grinding.
Embodiment 4:
Decolorization experiment
, decolour under 20 ℃, 50 ℃, 80 ℃ respectively to A method caramel, B method caramel with the product of embodiment 1,2,3 gained, the methyne orchid at room temperature decoloured,
The results are shown in the table.
Taken off thing A method caramel % B method caramel % methyne orchid
Temperature ℃ 20 50 80 20 50 80 room temperatures
Sample
Example 1 92 96 97 95 97 97 16ml
Example 2 90 93 95 93 96 96 14ml
Example 3 95 97 99 96 98 100 17ml

Claims (5)

1, a kind of preparation method of solid decolorizer is characterized in that:
(a) with drying after comminuted plants fibre material and the vitriol oil with 1: the weight ratio of 1-4 is mixed, and control reaction temperature 10-100 ℃, makes the material saccharification;
(b) saccharification liquid carries out charing under temperature 150-280 ℃ that limits and limiting time 10-100 minute condition;
(c) material that charing is good washes with water;
(d) dehydration;
(e) grind.
2, by the described method of claim 1, it is characterized in that said vegetable fibre material is plant material or the plant material of cellulose or their mixture that contains xylogen, the material mass dryness fraction is for containing moisture 5-10%(weight percent).
3, by the described method of claim 1, it is characterized in that the vegetable fibre material is 1 with the mixed weight ratio of the vitriol oil: 2.0-3.5.
4, by the described method of claim 1, it is characterized in that control reaction temperature 40-70 ℃.
5,, it is characterized in that 170-230 ℃ of carbonization temperature control, carbonization time 25-55 minute by the described method of claim 1.
CN 90104205 1990-06-06 1990-06-06 Process for preparing solid decolorizer Expired - Fee Related CN1022180C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 90104205 CN1022180C (en) 1990-06-06 1990-06-06 Process for preparing solid decolorizer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 90104205 CN1022180C (en) 1990-06-06 1990-06-06 Process for preparing solid decolorizer

Publications (2)

Publication Number Publication Date
CN1054754A CN1054754A (en) 1991-09-25
CN1022180C true CN1022180C (en) 1993-09-22

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Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100421793C (en) * 2006-11-10 2008-10-01 湖南师范大学 Method for preparing solid sulphoacid by catalyzing carbohydrate
CN105565313A (en) * 2015-12-25 2016-05-11 泰山医学院附属医院 Method for rapid preparation of medical activated carbon from ginkgo leaf
CN106904589A (en) * 2017-04-07 2017-06-30 华侨大学 A kind of hydro-thermal method prepares method and the application of bagasse Carbon Materials

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