CN1240220A - Process for preparing phenolic resin base globe activated char - Google Patents
Process for preparing phenolic resin base globe activated char Download PDFInfo
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- CN1240220A CN1240220A CN 98115717 CN98115717A CN1240220A CN 1240220 A CN1240220 A CN 1240220A CN 98115717 CN98115717 CN 98115717 CN 98115717 A CN98115717 A CN 98115717A CN 1240220 A CN1240220 A CN 1240220A
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- phenolic resin
- resin base
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- solidifying agent
- activated char
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Abstract
The preparation method of phenolic resin base global activated carbon is characterized by utilizing linear thermoplastic phenolic resin as raw material, and adding solidifying agent before globe formation. The process of oxidation non-melting for preparing asphalt base global activated carbon by using asphalt as raw material is omitted to attain the goal of reducing energy consumption and obtain the phenolic resin base global activated carbon whose grain size is about 2 mm and uniform. Said invention is simple in preparation process and low in energy consumption.
Description
The invention belongs to preparation method of active carbon, relate in particular to a kind of preparation method of phenolic resin base globe activated char.
Ball shape active carbon is owing to have good sphericity, higher mechanical properties, and tamped density is even when fixed bed uses, and helps fluid and at the uniform velocity passes through, and fluid resistance is little, and fluid pressure is fallen little.In addition, its adsorption desorption speed is fast.So obtained using widely in fields such as environmental protection, military affairs, medical treatment, chemical industry.Ball shape active carbon commonly used both at home and abroad at present is the asphalt-base spherical activated carbon that is set out and produced by pitch, and the operational path that is adopted as English Patent GB1468982 is:
1. coal, petroleum pitch are heat-treated at 200-400 ℃, generate tarry matters, remove wherein low molecule component by distillation or extraction then, its softening temperature is raise;
2. above-mentioned high softening point bitumen is mixed with aromatic solvent heating such as benzene, toluene, naphthalenes;
3. said mixture is dispersed in the dispersion medium of suspending agent-containing, in 50-350 ℃ of following balling-up, used suspension dispersive agent is water miscible macromolecular compounds such as half saponified polyvinyl ester, polyvinyl alcohol, methylcellulose gum;
4. the above-mentioned bitumen ball that contains aromatic solvent is immersed in and dissolves each other with aromatic solvent but do not have in the organic solvent extraction solution of affinity, extract aromatic solvent in the ball, obtain the micropore bitumen ball with pitch;
In oxidizing atmosphere with the following oxide treatment of micropore bitumen ball at 100-500 ℃, the bitumen ball oxidation is not melted, with prevent bitumen ball in carbonization process molten also;
In 500-1000 ℃ of scope with the charing under inert atmosphere protection of above-mentioned bitumen ball, and use steam activation, obtain asphalt-base spherical activated carbon.
Because the singularity of character of its raw material itself and the technology that is adopted, the manufacturing processed of this asphalt-base spherical activated carbon must have not melting process, promptly do not melt, make bitumen ball in carbonization process, be unlikely to the molten spherical carbon that also together can not get by oxidation.The technology that GB1468982 adopts does not melt the bitumen ball oxidation for the speed with (15-35 ℃)/hr is heated to 300 ℃ with bitumen ball in airflow.This process time consumption and energy consumption.This process belongs to gas-solid two-phase inhomogeneous reaction simultaneously, if sphere diameter is excessive, oxidation is not just melted and can not thoroughly be carried out.So the particle diameter of the asphalt-base spherical activated carbon of Zhi Zaoing is mostly between 0.1-1mm in this way.And the ball shape active carbon that uses in liquid phase adsorption for reducing the resistance of fluid flow, needs ball shape active carbon to have bigger particle diameter.
The document of producing ball shape active carbon with lacquer resins is few, and with the method that lacquer resins prepares thermoset microballoon such as Romanian patent Rom.Ro82.521 is:
With lacquer resins and hexamethylenetetramine with (75-95): ratio (5-25) is dissolved in methyl alcohol;
With chlorobenzene or kerosene with 1: the ratio (0.05-0.5) and the vinylbenzene of chlorosulphonation are mixed, stir;
3. mixture in 1 is added in 2, remains on 60 ℃ of following constant temperature 60min, to form dispersion;
4. be warmed up to 80 ℃ and remove methyl alcohol, constant temperature 180min obtains hardened ball;
5. keep 210min to obtain the resol microballoon of crosslinking curing down at 110-135 ℃.
Zhi Bei resol microspherulite diameter is difficult to control in this way, and size-grade distribution is inhomogeneous.
Goal of the invention of the present invention provides the preparation method of the phenolic resin base globe activated char that a kind of energy consumption is low, sphere diameter big and be evenly distributed.
The present invention realizes like this, utilize lacquer resins to be raw material, by before balling-up, adding solidifying agent, having saved is the oxidation melting process not of feedstock production asphalt-base spherical activated carbon with pitch, reach the purpose that energy consumption reduces, and obtain particle diameter about 2mm and the phenolic resin base globe activated char that is evenly distributed.
Preparation method of the present invention comprises the steps:
With lacquer resins with after solidifying agent mixes, make block mixture, block mixture is crushed to 1.25-2.5mm, obtains material resin;
2. material resin is distributed in the dispersion liquid that contains dispersion agent the emulsification balling-up;
3. the ball that is become is under protection of inert gas, is warmed up to 600-1000 ℃ with the speed of (1-20) ℃/min and carries out charing and handle;
4. the ball of charing processing utilizes water vapor or carbonic acid gas to carry out activation treatment under 700-900 ℃, obtains alkyd resin based ball shape active carbon;
It is characterized in that the described method of making block mixture has two kinds,
First method is with lacquer resins, solvent, solidifying agent is pressed lacquer resins: solvent: solidifying agent=1: (2-5): (0.06-0.15) proportioning of (weight ratio) is mixed, make lacquer resins and solidifying agent be dissolved in solvent, and stir, decompression steams solvent down, obtains block mixture;
Second method is with lacquer resins, solidifying agent is by lacquer resins: solidifying agent=1: (0.06-0.15) (weight ratio) carries out ball milling 30-90min under 0-40 ℃ of temperature, on press, be pressed into bulk then, and blow the edge of block with 300 ℃ warm air, make it to melt and become closely knit block mixture.
Described emulsification balling-up be with dispersion agent by dispersion agent: dispersion medium=(2-10): the proportioning of 100 (weight ratios) adds in the liquid dispersion medium that does not dissolve lacquer resins and forms dispersion liquid, material resin is pressed material resin: dispersion medium=(5-10): the proportioning of 100 (weight ratios) adds dispersion liquid, is warmed up to 90-140 ℃ and forms resin balls under at the uniform velocity stirring.
Aforesaid lacquer resins is the line style novolac resin of softening temperature between 60-120 ℃, and softening temperature is preferably between 95-120 ℃.
Aforesaid solvent is ethanol, methyl alcohol.
Aforesaid solidifying agent is hexamethylenetetramine, polyoxymethylene, preferably hexamethylenetetramine.
Aforesaid dispersion medium is water, glycerine, silicone oil, preferably water.
Aforesaid dispersion agent is a sodium lauryl sulphate, Emulsifier EL-90, Sudan Gum-arabic.
The present invention compared with prior art has following advantage:
1. step is simple, and energy consumption is low.
2. can obtain particle diameter is about 2mm, and the ball shape active carbon that is evenly distributed.
Embodiment 1
1. with 200 gram lacquer resinss, 400ml anhydrous methanol and 12 gram hexamethylenetetramines add in the reactor together, under 55 ℃, at the uniform velocity stirred 60 minutes, lacquer resins and hexamethylenetetramine are dissolved fully, then mixed solution is under reduced pressure steamed except that methyl alcohol, obtain block mixture, get particle diameter after the fragmentation between 1.25-2.5mm, be suitable for preparing the material resin of phenolic resin base globe activated char;
2. in autoclave, add 1000ml water, 30 gram sodium lauryl sulphate after stirring add resulting material resin 50 grams in 1, at the uniform velocity stir down and slowly are warmed up to 130 ℃, keep stirring to make the reactor naturally cooling, obtain the resol microballoon of particle diameter between 1.25-2.5mm;
3. the resol microballoon that obtains in the step 2 is heated to 900 ℃ and be incubated 30min and carry out charing with the speed of 2 ℃/min, obtains the resol based carbon microsphere;
4. the resol based carbon microsphere that obtains in the step 3 is heated to 900 ℃ with the speed of 10 ℃/min, feeds steam activation 15min, obtain phenolic resin base globe activated char, its particle diameter is at 1.0-2.3mm.The results are shown in Table 1.
Embodiment 2
1. mean particle size is put into ball mill jointly less than 200 purpose lacquer resinss, 1000 grams and polyoxymethylene 100 grams, keep the ball mill temperature between 0-30 ℃, to grind and mix 90min, on press, said mixture is pressed into piece then, blow the edge of block with 300 ℃ warm airs, make it to melt and become closely knit solids, be broken for particle diameter between 1.25-2.5mm, be suitable for preparing the material resin of phenolic resin base globe activated char;
2. add 700ml silicone oil in autoclave, 3 gram Emulsifier EL-90s stir, resulting material resin 40 grams in the step 1 are added, at the uniform velocity stir down and slowly be warmed up to 120 ℃, keep stirring to make the reactor naturally cooling, obtain the resol microballoon of particle diameter at 1.25-2.5mm;
Carry out charing as the step 3 among the embodiment 1,4 pairs of above-mentioned resol microballoons and handle, and, obtain phenolic resin base globe activated char at 900 ℃ of activation 30min.The results are shown in Table 1.
Embodiment 3
1. with 200 gram lacquer resinss, 400ml dehydrated alcohol and 30 gram hexamethylenetetramines add in the reactor together, under 60 ℃, at the uniform velocity stirred 60 minutes, lacquer resins and hexamethylenetetramine are dissolved fully, then mixed solution is under reduced pressure steamed except that ethanol, obtain block mixture, be broken for particle diameter between 1.25-2.5mm, be suitable for preparing the material resin of phenolic resin base globe activated char;
2. in autoclave, add 800ml water, 20 gram Sudan Gum-arabics, the back that stirs add resulting material resin 45 grams in the step 1, at the uniform velocity stir down and slowly are warmed up to 125 ℃, keep stirring to make the reactor naturally cooling, obtain the resol microballoon of particle diameter between 1.25-2.5mm;
Carry out charing as the step 3 among the embodiment 1,4 pairs of above-mentioned resol microballoons and handle, and, obtain phenolic resin base globe activated char at 900 ℃ of activation 15min.The results are shown in Table 1.
Comparative Examples 1
1. coal-tar middle oil pitch is heated to 350 ℃ in reactor, constant temperature 140 minutes blasts air simultaneously, makes the high softening point bitumen of softening temperature about 250 ℃:
2. with resulting high softening point bitumen 1000g in the step 1, naphthalene 250g adds in the autoclave that has agitator together, is heated to 270 ℃, evenly stirs to make it to mix, and is broken for the particle of 2～0.8mm after cooling;
3. add 10Kg distilled water in autoclave, the 4Kg polyvinyl alcohol stirs and makes it uniform mixing;
4. the pitch particle that obtains in the step 2 is joined in the dispersion liquid that obtains in the step 3,, obtain the pitch microballoon after the cooling, separate keeping stirring condition to be heated to 150 ℃;
5. the pitch microballoon that is 0.8-1.25mm with above-mentioned isolated particle diameter is put into thermostatic drying chamber, blasts air and is heated to 280 ℃ with the speed of 0.5 ℃/min, and constant temperature 3 hours obtains not molten asphalt ball;
6. the speed with 3 ℃/min is heated to 900 ℃ with above-mentioned insoluble bitumen ball under nitrogen protection, and constant temperature 30min carries out the charing processing;
7. feed steam activation 30min down at 900 ℃, obtain asphalt-base spherical activated carbon.The results are shown in Table 1.
Comparative Examples 2
As described in Comparative Examples 1, the pitch microballoon of the 4th isolated particle diameter of step between 1.25-2mm in the Comparative Examples 1 carried out similar processing, found that in carbonization process subsequently the pitch microballoon is molten also together.The character of table 1 gained phenolic aldehyde base globe activated char reaches the contrast with asphalt-base spherical activated carbon
| Classification | Particle diameter (mm) | BET specific surface area (m 2/g) | Micropore specific surface (m 2/g) | Total pore volume cm 3/g | Micropore pore volume (cm 3/g) | Mean pore size () |
| Phenolic resin base globe activated char soak time 15min among the embodiment 1 | ??2.3-1.0 | ????657 | ??556 | ????0.35 | ????0.29 | ????14.7 |
| Phenolic resin base globe activated char soak time 30min among the embodiment 2 | ??2.3-1.0 | ????1045 | ??792 | ????0.58 | ????0.42 | ????14.6 |
| Phenolic resin base globe activated char soak time 15min among the embodiment 3 | ??2.3-1.0 | ????605 | ??512 | ????0.29 | ????0.24 | ????14.4 |
| Comparative Examples 1 medium pitch base globe activated char soak time 30min | ??0.6-1.0 | ????730 | ??605 | ????0.37 | ????0.29 | ????13.5 |
| Comparative Examples 2 medium pitch microballoons | Melt also |
Claims (9)
1. the preparation method of a phenolic resin base globe activated char comprises the steps:
(1) with lacquer resins with after solidifying agent mixes, make block mixture, block mixture is crushed to 1.25-2.5mm, obtains material resin;
(2) material resin is distributed in the dispersion liquid that contains dispersion agent the emulsification balling-up;
(3) ball that is become is under protection of inert gas, is warmed up to 600-1000 ℃ with the speed of (1-20) ℃/min and carries out charing and handle;
(4) ball of charing processing utilizes water vapor or carbonic acid gas to carry out activation treatment under 700-900 ℃, obtains alkyd resin based ball shape active carbon;
It is characterized in that the described method of making block mixture has two kinds:
First method is with lacquer resins, solvent, solidifying agent is pressed lacquer resins: solvent: solidifying agent=1: (2-5): (0.06-0.15) proportioning of (weight ratio) is mixed, make lacquer resins and solidifying agent be dissolved in solvent, and stir, decompression steams solvent down, obtains block mixture;
Second method is with lacquer resins, solidifying agent is by lacquer resins: solidifying agent=1: (0.06-0.15) (weight ratio) mixed the back and carried out under 0-40 ℃ of temperature ball milling 30-90 minute, on press, be pressed into bulk then, and blow the edge of block with 300 ℃ warm air, make it to melt and become closely knit block mixture;
Described emulsification balling-up be with dispersion agent by dispersion agent: dispersion medium=(2-10): the proportioning of 100 (weight ratios) adds in the liquid dispersion medium that does not dissolve lacquer resins and forms dispersion liquid, material resin is pressed material resin: dispersion medium=(5-10): the proportioning of 100 (weight ratios) adds dispersion liquid, is warmed up to 90-140 ℃ of formation microballoon under at the uniform velocity stirring.
2. the preparation method of a kind of phenolic resin base globe activated char according to claim 1 is characterized in that described resol is the line style novolac resin of softening temperature between 60-120 ℃.
3. the preparation method of a kind of phenolic resin base globe activated char according to claim 1 and 2 is characterized in that described resol softening temperature is preferably between 95-120 ℃.
4. the preparation method of a kind of phenolic resin base globe activated char according to claim 1 is characterized in that described solvent is ethanol, methyl alcohol.
5. the preparation method of a kind of phenolic resin base globe activated char according to claim 1 is characterized in that described solidifying agent is hexamethylenetetramine, polyoxymethylene.
6. a kind of preparation method of phenolic resin base globe activated char according to claim 1 or 5 is characterized in that described solidifying agent is to be preferably hexamethylenetetramine.
7. the preparation method of a kind of phenolic resin base globe activated char according to claim 1 is characterized in that described dispersion medium is water, glycerine, silicone oil.
8. according to the preparation method of claim 1 or 7 described a kind of phenolic resin base globe activated chars, it is characterized in that preferably water of described dispersion medium.
9. the preparation method of a kind of phenolic resin base globe activated char according to claim 1 is characterized in that described dispersion agent is a sodium lauryl sulphate, Emulsifier EL-90, Sudan Gum-arabic.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98115717A CN1075539C (en) | 1998-06-24 | 1998-06-24 | Process for preparing phenolic resin base globe activated char |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98115717A CN1075539C (en) | 1998-06-24 | 1998-06-24 | Process for preparing phenolic resin base globe activated char |
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| CN1240220A true CN1240220A (en) | 2000-01-05 |
| CN1075539C CN1075539C (en) | 2001-11-28 |
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| CN98115717A Expired - Fee Related CN1075539C (en) | 1998-06-24 | 1998-06-24 | Process for preparing phenolic resin base globe activated char |
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| CN100453458C (en) * | 2007-03-20 | 2009-01-21 | 中国科学院山西煤炭化学研究所 | Preparation method of lightweight heat-proof phenolic resin radical foam charcoal |
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Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RO82521A2 (en) * | 1981-06-26 | 1983-10-15 | Institutul De Chimie Macromoleculara "P.Poni",Ro | PROCESS FOR OBTAINING PEARL SHAPED RESIDENCES |
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1998
- 1998-06-24 CN CN98115717A patent/CN1075539C/en not_active Expired - Fee Related
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