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: