CN102247806B - Activated carbon for solvent recovery produced from wood materials and preparation method thereof - Google Patents
Activated carbon for solvent recovery produced from wood materials and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an activated carbon for solvent recovery produced from wood materials and a preparation method thereof. The activated carbon for solvent recovery is characterized by simple production process, wide raw material resource, reduced production cost, superior product performance and strong competitiveness. The method comprises a plurality of processing steps such as raw material mixing, pre-carbonization (slaking), granulation, drying, screening, pre-activation, activation, catalyst recovery, rinsing and drying, etc. With simple production process, the activated carbon of the invention can be obtained by processing well proportioned raw materials. The activated carbon of the invention has wide raw material resources and reduced production cost, so that the price of a final product can be reduced and the market competitiveness can be improved. The characteristics of high adsorption capacity, high intensity, easy desorption, wide application scope and the like in theproduct itself can further improve the product market competitiveness.
Description
Technical field
The present invention relates to a kind of solvent recovery active carbon and preparation method who produces with wood materials.
Background technology
Active carbon can be traced back to eighties of last century the forties in the history that chemical industry, petrochemical industry, light industry carry out solvent recovery, and the extensive use of China's solvent recovery active carbon starts from the eighties of last century the eighties.Past mainly is squeezed into column or sphere with low grey fine coal coal tar, pitch, makes through the Physical activation.This technique still is the main product of solvent recovery at present.But because this technique is subjected to the restriction of raw material and technique itself, can't make the product of low ash content (＜5%), high-performance (carbon tetrachloride〉100%), can not satisfy existing market to the demand of quality and range of application.The domestic manufacturing enterprise that there is no the wooden solvent recovery active carbon of formation scale production capacity did not meet the associated authorization patent of producing the solvent active carbon with wood materials yet at present.Solvent recovery active carbon high-quality and specific use mainly relies on external import at present, because the product price of external import is relatively high, causes enterprise to increase production cost, and then the price of the product that relies on this solvent production is raise.At present also have no the Patents that has relevant enterprise to apply at home abroad authorized.
Summary of the invention
The object of the present invention is to provide a kind of 1, production process is simple, 2, raw material resources extensively, lower the cost of production, 3, properties of product are superior, competitiveness is strong.
The object of the present invention is achieved like this: it may further comprise the steps:
(1) raw material mixes: the environment of wood powder and catalyst by proportion being put into 80-125 ℃ stirs 20～40 minutes to mixing;
(2) pre-charing (slaking): the mixture of step (1) is being carried out carrying out pre-charing at 100 ~ 170 ℃ after the drying, and the time of pre-charing is 10-15 hour;
(3) granulation: the product that step (2) is obtained was fully mediated 40-70 minute after adding catalyst, and the material after the kneading carries out granulation in forming machine;
(4) drying: the particle in the step (3) placed 120 ± 5 ℃ the dry 80-160 of environment minute;
(5) screening: the product of step (4) is screened by the standard of screening;
(6) the pre-activation: the environment of the qualified material of step (5) being put into 140 ~ 250 ℃ activates in advance, and the preactivated time is 6 ~ 24 hours;
(7) activate: the environment of the product of step (6) being put into 380-540 ℃ activates, and the time of activation is 20-80 minute;
(8) catalyst recovery: the product of step (7) is carried out catalyst recovery, reclaim to adopt mode that adverse current reclaims catalyst content＜1% to the solution;
(9) rinsing: adopt clear water to carry out rinsing until the pH value of product is 3 product of step (8);
(10) oven dry: the product that step (9) obtains is dried in baking oven, and bake out temperature is controlled at 120-140 ℃, and time 2-4 hour, the product moisture after the oven dry is controlled at＜and 3%.
The solvent recovery active carbon that production technology of the present invention is produced comprises 2 types of column structure and chondritics; Wherein, column structure is diameter ￠ 1.5-4mm, and chondritic is the 4-80 order, the intensity 80-99% of column structure, the intensity 60-85% of chondritic; The carbon tetrachloride adsorption rate 100-140% of column structure, the carbon tetrachloride adsorption rate 100-160% of chondritic.
Advantage of the present invention is as follows: 1, production process is simple, by the good raw material of proportioning are processed and can be obtained; 2, raw material resources extensively, reduced the cost of production, thereby final product price is reduced, improve the market competitiveness; 3, product itself has high-adsorption-capacity, high strength, and easily desorb, the characteristics such as applied widely can further improve the competitiveness of product in market.
The specific embodiment
Mainly it may further comprise the steps in the present invention:
(1) raw material mixes: the environment of wood powder and catalyst by proportion being put into 80-125 ℃ stirs 20～40 minutes to mixing; The ratio of wherein mixing is that the weight ratio of mixing between wood powder and the catalyst is 1:0.8-2.0.
Wood powder in the raw material is for being crushed to the wood powder of 20～100 orders, moisture 5～20% after one or more mixing in coconut husk, apricot shell, tea seed shell, industrial wood shavings, the sawdust; Described catalyst is any one solution in phosphoric acid, zinc chloride, calcium chloride, sulfuric acid, boric acid, potassium bichromate, the potassium permanganate, and the concentration of solution is 30-70%; During as catalyst, the properties of product that obtain are best with phosphoric acid, zinc chloride for described catalyst.
(2) pre-charing (slaking): the mixture of step (1) was carried out drying in 10-15 hour 80-125 ℃ of lower the placement.Carrying out carrying out pre-charing at 100 ~ 170 ℃ after the drying, the time of pre-charing is 10-15 hour; (3) granulation: the product that step (2) is obtained was fully mediated 40-70 minute after adding catalyst, and the material after the kneading carries out granulation in forming machine; The forming machine here is generally the spherical forming machine of drum-type or extruded type forming machine.Carry out granulation according to different forming machines.
(4) drying: the particle in the step (3) placed 120 ± 5 ℃ the dry 80-160 of environment minute;
(5) screening: the product of step (4) is screened by the standard of screening;
(6) the pre-activation: the environment of the qualified material of step (5) being put into 140 ~ 250 ℃ activates in advance, and the preactivated time is 6 ~ 24 hours; Wherein, the preactivated temperature of material take 160～180 ℃ as optimum temperature range, the preactivated time is take 15～20 hours as the Best Times scope.
(7) activate: the environment of the product of step (6) being put into 380-540 ℃ activates, and the time of activation is 20-80 minute; Wherein, the temperature of material activating take 450～500 ℃ as optimum temperature range, the preactivated time is take 2～3 hours as the Best Times scope.
(8) catalyst recovery: the product of step (7) is carried out catalyst recovery, reclaim to adopt mode that adverse current reclaims catalyst content＜1% to the solution;
(9) rinsing: adopt clear water to carry out rinsing until the pH value of product is 3 product of step (8);
(10) oven dry: the product that step (9) obtains is dried in baking oven, and bake out temperature is controlled at 120-140 ℃, and time 2-4 hour, the product moisture after the oven dry is controlled at＜and 3%.
In order to be the last uniform specification of product, in general, the product after the oven dry of the product of production also needs through screening, detects.
The step of product is illustrated as follows:
The solvent recovery active carbon that this production technology is produced comprises 2 types of column structure and chondritics; Wherein, column structure is diameter ￠ 1.5-4mm, and chondritic is the 4-80 order, the intensity 80-99% of column structure, the intensity 60-85% of chondritic; The carbon tetrachloride adsorption rate 100-140% of column structure, the carbon tetrachloride adsorption rate 100-160% of chondritic.
Wherein, spherical products can be subdivided into again 4 types in 4-14 order, 14-25 order, 25-50 order, 50-80 order.
Below in conjunction with specific embodiment this preparation method and products thereof feature is described:
The order number average of the wood materials that adopts is the 30-80 order.
Selecting phosphoric acid in the case 1～3 is catalyst.
Case 1: select order to count 30-80 order wood powder 1000g, the phosphoric acid solution 1300ml of adding 70%, in the jacket type stirring machine, mix after 30 minutes, 120 ℃ ± 2 ℃ of jacket temperatures, mixed material dislocation enters drying box, promote after lower dry 15 hours under 160-170 ℃ of the temperature at 125 ℃ and to carry out pre-charing, pre-carbonization time 15 hours.Material after the pre-charing moves in the kneading machine, adds 15% phosphoric acid solution 150ml, fully kneads 60 minutes.The moulding in the extruded type forming machine of material after kneading obtains ￠ 4.8mm product, and is for subsequent use with 120 minutes laggard row filters of 120 ℃ ± 5 ℃ dryings in drying box.Product after the screening is put in the electric furnace and is activated in advance, 245 ℃ ± 2 ℃ of pre-activation temperatures, 12 hours time.Promote subsequently temperature to 430 ℃ ± 5 ℃, keep taking out after 20 minutes, the product after the activation is carried out phosphoric acid reclaim, and rinsing is to pH value 3, oven dry obtains product 375g 140 ℃ of lower oven dry 3 hours after the screening.It is as follows that product detects data:
Case 2: select order to count 30-80 order wood powder 1000g, the phosphoric acid solution 1400ml of adding 60%, in the jacket type stirring machine, mix after 30 minutes, 120 ℃ ± 2 ℃ of jacket temperatures, mixed material dislocation enters drying box, promote after lower dry 20 hours under 160-170 ℃ of the temperature at 125 ℃ and to carry out pre-charing, pre-carbonization time 12 hours.Material after the pre-charing moves in the kneading machine, adds 15% phosphoric acid solution 150ml, fully kneads 60 minutes.The moulding in the extruded type forming machine of material after kneading obtains ￠ 3.6mm product, and is for subsequent use with 120 minutes laggard row filters of 120 ℃ ± 5 ℃ dryings in drying box.Product after the screening is put in the electric furnace and is activated in advance, 265 ℃ ± 5 ℃ of pre-activation temperatures, 16 hours time.Promote subsequently temperature to 520 ℃ ± 5 ℃, keep taking out after 30 minutes, the product after the activation is carried out phosphoric acid reclaim, and rinsing is to pH value 3, oven dry obtains product 355g 120 ℃ of lower oven dry 4 hours after the screening.It is as follows that product detects data:
Case 3: select order to count 30-80 order wood powder 1000g, the phosphoric acid solution 1300ml of adding 70%, in the jacket type stirring machine, mix after 30 minutes, 120 ℃ ± 2 ℃ of jacket temperatures, mixed material dislocation enters drying box, promote after lower dry 15 hours under 160-170 ℃ of the temperature at 125 ℃ and to carry out pre-charing, pre-carbonization time 15 hours.Material after the pre-charing moves in the kneading machine, adds 15% phosphoric acid solution 150ml, fully kneads 60 minutes.The moulding in the spherical forming machine of drum-type of material after kneading obtains ￠ 4-12 order product, and is for subsequent use with 120 minutes laggard row filters of 120 ℃ ± 5 ℃ dryings in drying box.Product after the screening is put in the electric furnace and is activated in advance, 245 ℃ ± 2 ℃ of pre-activation temperatures, 12 hours time.Promote subsequently temperature to 450 ℃ ± 5 ℃, keep taking out after 20 minutes, the product after the activation is carried out phosphoric acid reclaim, and rinsing is to pH value 3, oven dry obtains product 340g 120 ℃ of lower oven dry 4 hours after the screening.It is as follows that product detects data:
Case 4: select order to count 30-80 order wood powder 1000g, the ZnCl2 solution 800ml of adding 70%, in the jacket type stirring machine, mix after 20 minutes, 82 ℃ ± 2 ℃ of jacket temperatures, mixed material dislocation enters drying box, promote after lower dry 10 hours under 160-170 ℃ of the temperature at 80 ℃ and to carry out pre-charing, pre-carbonization time 6 hours.Material after the pre-charing moves in the kneading machine, adds 15% ZnCl2 solution 150ml, fully kneads 40 minutes.The moulding in the extruded type forming machine of material after kneading obtains ￠ 4.8mm product, and is for subsequent use with 80 minutes laggard row filters of 120 ℃ ± 5 ℃ dryings in drying box.Product after the screening is put in the electric furnace and is activated in advance, 245 ℃ ± 2 ℃ of pre-activation temperatures, 6 hours time.Promote subsequently temperature to 535 ℃ ± 5 ℃, keep taking out after 20 minutes, the product after the activation is carried out ZnCl2 reclaim, and rinsing is to pH value 3, oven dry obtains product 345g 120 ℃ of lower oven dry 3 hours after the screening.It is as follows that product detects data:
Case 4: select order to count 30-80 order wood powder 1000g, the ZnCl2 solution 2000ml of adding 60%, in the jacket type stirring machine, mix after 40 minutes, 82 ℃ ± 2 ℃ of jacket temperatures, mixed material dislocation enters drying box, promote after lower dry 15 hours under 160-170 ℃ of the temperature at 80 ℃ and to carry out pre-charing, pre-carbonization time 15 hours.Material after the pre-charing moves in the kneading machine, adds 15% ZnCl2 solution 150ml, fully kneads 40 minutes.The moulding in the extruded type forming machine of material after kneading obtains ￠ 4.8mm product, and is for subsequent use with 160 minutes laggard row filters of 120 ℃ ± 5 ℃ dryings in drying box.Product after the screening is put in the electric furnace and is activated in advance, 142 ℃ ± 2 ℃ of pre-activation temperatures, 24 hours time.Promote subsequently temperature to 38 ℃ ± 5 ℃, keep taking out after 80 minutes, the product after the activation is carried out ZnCl2 reclaim, and rinsing is to pH value 3, oven dry obtains product 345g 140 ℃ of lower oven dry 4 hours after the screening.It is as follows that product detects data:
Claims (10)
1. the preparation method of a solvent recovery active carbon of producing with wood materials, it is characterized in that: it may further comprise the steps:
(1) raw material mixes: the environment of wood powder and catalyst by proportion being put into 80-125 ℃ stirs 20～40 minutes to mixing;
(2) pre-charing: the mixture of step (1) is being carried out carrying out pre-charing at 100～170 ℃ after the drying, and the time of pre-charing is 10-15 hour;
(3) granulation: the product that step (2) is obtained was fully mediated 40-70 minute after adding the catalyst that weight is wood powder gross weight 15%, and the material after the kneading carries out granulation in forming machine;
(4) drying: the particle in the step (3) placed 120 ± 5 ℃ the dry 80-160 of environment minute;
(5) screening: the product of step (4) is screened by the standard of screening;
(6) the pre-activation: the environment of the qualified material of step (5) being put into 140～250 ℃ activates in advance, and the preactivated time is 6～24 hours;
(7) activate: the environment of the product of step (6) being put into 380-540 ℃ activates, and the time of activation is 20-80 minute;
(8) catalyst recovery: the product of step (7) is carried out catalyst recovery, reclaim to adopt mode that adverse current reclaims catalyst content＜1% to the solution;
(9) rinsing: adopt clear water to carry out rinsing until the pH value of product is 3 product of step (8);
(10) oven dry: the product that step (9) obtains is dried in baking oven, and bake out temperature is controlled at 120-140 ℃, and time 2-4 hour, the product moisture after the oven dry is controlled at＜and 3%.
2. the preparation method of the solvent recovery active carbon of producing with wood materials according to claim 1, it is characterized in that: the weight ratio of mixing between wood powder and the catalyst is 1:0.8-2.0.
3. the preparation method of the solvent recovery active carbon of producing with wood materials according to claim 1 is characterized in that: the wood powder described in the step 1 for will be in coconut husk, apricot shell, tea seed shell, industrial wood shavings, the sawdust one or more be crushed to the wood powder of 20～100 orders, moisture 5～20% after mixing; Described catalyst is any one solution in phosphoric acid, zinc chloride, calcium chloride, sulfuric acid, boric acid, potassium bichromate, the potassium permanganate, and the concentration of solution is 30-70%.
4. the preparation method of the solvent recovery active carbon of producing with wood materials according to claim 3 is characterized in that: during as catalyst, the properties of product that obtain are best with phosphoric acid, zinc chloride for described catalyst.
5. the preparation method of the solvent recovery active carbon of producing with wood materials according to claim 1, it is characterized in that: mixture is to carry out drying in 10-15 hour 80-125 ℃ of lower the placement in the step (2).
6. the preparation method of the solvent recovery active carbon of producing with wood materials according to claim 1, it is characterized in that: the forming machine in the step (3) is the spherical forming machine of drum-type or extruded type forming machine.
7. the preparation method of the solvent recovery active carbon of producing with wood materials according to claim 1, it is characterized in that: in the step (6), the preactivated temperature of material take 160～180 ℃ as optimum temperature range, the preactivated time is take 15～20 hours as the Best Times scope.
8. the preparation method of the solvent recovery active carbon of producing with wood materials according to claim 1, it is characterized in that: the product after the oven dry also needs through screening, detects.
9. the prepared solvent recovery active carbon of the described preparation method of any one claim in 8 according to claim 1 is characterized in that: comprise 2 types of column structure and chondritics; Wherein, column structure is diameter ￠ 1.5-4mm, and chondritic is the 4-80 order, the intensity 80-99% of column structure, the intensity 60-85% of chondritic; The carbon tetrachloride adsorption rate 100-140% of column structure, the carbon tetrachloride adsorption rate 100-160% of chondritic.
10. active carbon according to claim 9 is characterized in that: spherical products can be subdivided into again 4 types in 4-14 order, 14-25 order, 25-50 order, 50-80 order.
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| US10259714B2 (en) | 2015-03-19 | 2019-04-16 | The University Of Akron | Method of making mesoporous carbon from natural wood and mesoporous carbon hollow tubes made thereby |
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| CN103464100B (en) * | 2013-09-06 | 2016-04-27 | 济南圣泉集团股份有限公司 | The method of solvent recovery active carbon adsorption material is prepared by plant acidolysis slag |
| CN105080485A (en) * | 2015-09-29 | 2015-11-25 | 江苏锦宇环境工程有限公司 | Method for preparing carbon bio-adsorbent from Chinese parasol fallen leaves |
| CN106512944A (en) * | 2016-12-06 | 2017-03-22 | 福建师范大学 | Production method of oxidized wood active carbon for effectively adsorbing carbon dioxide |
| CN111170319A (en) * | 2020-02-15 | 2020-05-19 | 太原理工大学 | Method for preparing high-performance activated carbon for automobile carbon tank by using mycelia |
| CN115818642A (en) * | 2022-12-09 | 2023-03-21 | 南平元力活性炭有限公司 | Production method of self-bonding high-strength wood columnar activated carbon |
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| CN1528510A (en) * | 2003-09-26 | 2004-09-15 | 鹏 林 | Vehicular wood active carbon and preparing method tehreof |
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| CN101407323B (en) * | 2008-09-16 | 2011-05-18 | 上海第二工业大学 | Method for preparing pressed active carbon from tobacco stalk |
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| CN1528510A (en) * | 2003-09-26 | 2004-09-15 | 鹏 林 | Vehicular wood active carbon and preparing method tehreof |
Cited By (1)
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| US10259714B2 (en) | 2015-03-19 | 2019-04-16 | The University Of Akron | Method of making mesoporous carbon from natural wood and mesoporous carbon hollow tubes made thereby |
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Denomination of invention: Activated carbon for solvent recovery produced from wood materials and preparation method thereof Effective date of registration: 20151231 Granted publication date: 20131016 Pledgee: Industrial Commercial Bank of China Ltd. Shaowu branch Pledgor: FUJIAN XINSEN CARBON Co.,Ltd. Registration number: 2015350000114 |
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