CN102464792B - Method and device for reducing volatile matters of o-cresol-formaldehyde epoxy resin - Google Patents
Method and device for reducing volatile matters of o-cresol-formaldehyde epoxy resin Download PDFInfo
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- CN102464792B CN102464792B CN 201010552018 CN201010552018A CN102464792B CN 102464792 B CN102464792 B CN 102464792B CN 201010552018 CN201010552018 CN 201010552018 CN 201010552018 A CN201010552018 A CN 201010552018A CN 102464792 B CN102464792 B CN 102464792B
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Abstract
The invention discloses a method and device for reducing volatile matters of an o-cresol-formaldehyde epoxy resin. The method comprises the following step of: performing a two-stage desolventizing step, including a coarse desolventizing step and a fine desolventizing step to remove a solvent and a high-boiling residue component from an o-cresol-formaldehyde epoxy resin. The device comprises a feed pump, a first pipeline mixer, a falling film evaporator, a gas-liquid separator, a primary removal extraction pump, a second pipeline mixer, a thin-film evaporator, a packing tower and a secondary removal extraction pump which are connected in sequence, wherein a part of an o-cresol-formaldehyde epoxy resin solution output by the gas-liquid separator returns to the first pipeline mixer through a reflux pump; a steam inlet/outlet is formed in the second pipeline mixer; and both the gas-liquid separator and a film evaporator are provided with a volatile matter gas-phase outlet. According to the method and the device for reducing the volatile matters of the o-cresol-formaldehyde epoxy resin, volatile matters of a product can be reduced to be below 0.05 percent, and the performance of the product applied to an electronic molding compound can be improved remarkably.
Description
Technical field
The present invention relates to a kind of method and apparatus that reduces the o-cresol formaldehyde epoxy resin fugitive constituent.
Technical background
Along with the development of electronic industry technology, the demand of unicircuit packaged material is increasing severely, and its main application has: computer, the network equipment, automatic control device, communication apparatus and consumer electronics product etc.Be the needs of the multifunction that adapts to these products, light, thin, short and smallization, electronic devices and components move towards gradually that integrated scale super largeization, wiring width nanometer, package dimension microminiaturization, element are installed densification and process automation, element is installed automatization.The needs that be to adapt to densification to not producing defective such as micro-bubble in the components and parts packaged material course of processing, reduce the components and parts failure rate as far as possible, require the Resins, epoxy base material to have enough low volatizable material content.
Mainly comprise residual solvent that manufacturing processed produces, high boiling point by-products produced, moisture etc. in the o-cresol formaldehyde epoxy resin fugitive constituent.Wherein the content of residual solvent and moisture is easier to separate in the resin, what usually adopt is to heat up and be aided with by decompression to make the film forming method of resin make it gasification to separate, and it is high boiling point by-products produced because of its complicated component, the boiling point of some components is much higher than the boiling point of solvent, is difficult to separate from resin under same processing condition.In the prior art, the removal methods and the device of residual volatile component in a kind of polymer system have only been reported at patent CN1167772, adopt and become big well heater step by step, the devolatilization groove of built-in heating sparger, stirring rake and grid distributor, polymkeric substance is behind the multistage well heater of expansible step by step, enter the devolatilization groove, slough residual volatile component through separator again.In addition, do not see the relevant method of epoxy resin product fugitive constituent or the patent of device of reducing.
Summary of the invention
Technical problem to be solved by this invention is to propose a kind of method and apparatus that reduces the o-cresol formaldehyde epoxy resin fugitive constituent, the method and apparatus of this reduction o-cresol formaldehyde epoxy resin fugitive constituent can be reduced to the product fugitive constituent below 0.05% (weight), product odour also has obvious decline simultaneously, when product is used for the electronics plastic cement, can not reduce greatly because of air bubble problem causes the components and parts failure rate, performance be improved significantly.
Technical solution of the present invention is as follows:
A kind of method that reduces the o-cresol formaldehyde epoxy resin fugitive constituent adopts thick desolventizing step and smart desolventizing step two-stage desolventizing step to slough solvent and high boiling material component in the o-cresol formaldehyde epoxy resin;
Described thick desolventizing step is: o-cresol formaldehyde epoxy resin solution is sent in first line mixer, pass through falling-film evaporator and gas-liquid separator again, with the solvent in the preliminary removal o-cresol formaldehyde epoxy resin solution, removed solvent is discharged from gas-liquid separator with volatile matter gas phase form, the liquid phase part of gas-liquid separator output turns back in first line mixer by reflux pump, and another part takes off extractor pump by one and enters smart desolventizing step; The solvent of being removed through thick desolventizing step accounts for more than 99% of total solvent quality;
Described smart desolventizing step is: the o-cresol formaldehyde epoxy resin solution that passes through thick desolventizing step process enters to pass through successively after the mixing in second line mixer with steam again and steams film evaporator and packing tower, take off extractor pump by two at last and discharge, in luwa evaporator and packing tower, slough remaining solvent and high boiling material composition.
The effect of packing tower is to increase the resin solution specific surface area, prolongs the resin solution residence time.
In packing tower, adopt hot nitrogen treatment technology to increase the removal efficiency of volatilizable thing.
Falling-film evaporator is vertical adverse current falling-film evaporator; The falling-film evaporator heating medium adopts the following low-pressure steam of 2.5Mpa.
Described thin-film evaporator is a luwa evaporator, and luwa evaporator is vertical movable scraping plate formula vaporizer, and the luwa evaporator heating medium is a thermal oil, and azeotrope adopts the following low-pressure steam of 2.5Mpa, and hot nitrogen temperature is controlled at 80～120 ℃.
In the thick desolventizing step, temperature is controlled at 90～180 ℃; The vacuum degree control of the device of thick desolventizing step correspondence is at 5～25kPa.
In the smart desolventizing step, the vacuum degree control of the device of smart desolventizing step correspondence is at 0.5～5kPa, and temperature is controlled at 90～180 ℃.
Thin-film evaporator comprises and rises film, falling liquid film and luwa evaporator, and film is big class, and knifing is a group, so determine it is knifing.
The filler of filling in first line mixer and second line mixer is Pall ring, Raschig ring or cascade ring, the filler mode is for huddling, the filler of filling in the packing tower is Pall ring, Raschig ring or cascade ring, and the filler mode is for huddling, and the system feeding amount is for greater than 0 and be less than or equal to 20L/min.
A kind of device that reduces the o-cresol formaldehyde epoxy resin fugitive constituent, fresh feed pump, first line mixer, falling-film evaporator, gas-liquid separator, take off extractor pump, second line mixer, thin-film evaporator, packing tower and two and take off extractor pump and link to each other successively, some turns back to the o-cresol formaldehyde epoxy resin solution of gas-liquid separator output in first line mixer through reflux pump, in second line mixer, be provided with the steam admission port, on gas-liquid separator and thin-film evaporator, be equipped with the volatile matter gaseous phase outlet.
Described packing tower is provided with and is used for the inlet that hot nitrogen enters.
Described thin-film evaporator is a luwa evaporator.
Beneficial effect:
Compared with prior art, the present invention has following tangible advantage:
The horizontal pipeline mixing tank that the present invention uses is the material of two kinds of different viscosity of uniform mixing well, make that the material film forming that enters falling-film evaporator is even, improve the effect that refluxes and handle again, has the effect that improves feeding temperature simultaneously, improve the desolventizing efficient of slightly taking off level greatly, the solvent removal rate that guarantees slightly to take off level is stablized the operating mode that essence is taken off level well more than 99%.
The riser mixing tank that the present invention uses makes water vapor and resin coflow, discharges with volatilizable thing one homocoagulation in condenser through luwa evaporator.Can make resin at the filling surface uniform distribution, make water vapor uniform distribution in packing layer, uniform mixing resin and water vapor increase the gas-to-liquid contact area, increase residual high boiling material generation azeotropic efficient in water vapor and the resin, thereby increase the decreasing ratio of high boiling material.
The packing tower that the present invention uses makes through heated nitrogen and resin countercurrent flow, discharges from the vacuum pump venting port through luwa evaporator.It is long-pending to increase the resin film formation surface well, improves greatly and conducts heat and mass-transfer efficiency, improves the rate of volatilization of volatilizable thing, thereby effectively reduces the fugitive constituent of rosin products, improves plant capacity.
That uses among the present invention slightly takes off the level treatment technology that refluxes again and can improve the falling-film evaporator feeding temperature, is aided with the line mixer technology, can improve the film-formation result of falling-film evaporator greatly, thereby improve solvent removal efficient.
The water vapor azeotropic technology of using among the present invention utilizes water vapor to increase the total vapour pressure of mixed gas, reduce the boiling point of mixed gas, increase the gasification efficiency of volatilizable thing in the resin, thereby under the constant situation of process conditions, improve the removal efficiency of volatilizable thing.
The hot nitrogen treatment technology utilization that the present invention uses increases the total vapour pressure of mixed gas through heated nitrogen, reduce the boiling point of mixed gas, increase the gasification efficiency of volatilizable thing in the resin, thereby under the constant situation of process conditions, improve the removal efficiency of volatilizable thing.
The present invention compared with prior art, use moulding horizontal pipeline mixing tank, riser gas mixture and packing tower simple, with low cost, improved the removal efficiency of volatilizable thing, having solved prior art need increase the difficult problem that one or more levels vaporizer could reduce fugitive constituent.
Description of drawings
Fig. 1 is a horizontal pipeline mixer structure synoptic diagram;
Fig. 2 is a riser mixer structure synoptic diagram;
Fig. 3 is the packing tower structural representation;
Fig. 4 is the method and apparatus synoptic diagram of reduction o-cresol formaldehyde epoxy resin fugitive constituent of the present invention.
Label declaration: label: 1-two takes off extractor pump, 2-fresh feed pump, 3-first line mixer, 4-falling-film evaporator, 5-gas-liquid separator, the 6-reflux pump, 7-one takes off extractor pump, 8-second line mixer, 9-luwa evaporator, the 10-packing tower, A-charging, B-volatile matter gas phase, C-steam.
Embodiment
Below with reference to figure and specific implementation process the present invention is described in further details:
Embodiment 1:
Horizontal pipeline mixer structure, riser mixer structure and packing tower structure are respectively as Figure 1-3.
Filler in the horizontal pipeline mixing tank can make the liquid phase of backflow and the material uniform mixing of two kinds of different viscosity of resin solution, makes that the material film forming that enters falling-film evaporator is even, improves the effect that refluxes and handle, has the effect that improves feeding temperature simultaneously.
The riser mixing tank makes water vapor and resin coflow, discharges with volatilizable thing one homocoagulation in condenser through luwa evaporator.
Packing tower makes through heated nitrogen and resin countercurrent flow, discharges from the vacuum pump venting port through luwa evaporator.
The method and apparatus of reduction o-cresol formaldehyde epoxy resin fugitive constituent of the present invention is used for 2kt/a o-cresol formaldehyde epoxy resin device, and the process flow sheet that provides by Fig. 4 carries out the device design.In the actual production, 90～180 ℃ of first step service temperatures, first step vacuum tightness 5～25kPa, 90～180 ℃ of second stage service temperatures, second stage vacuum tightness 0.5～5kPa.The system feeding amount is respectively 8L/min and 18L/min, and the product fugitive constituent detected result that obtains sees Table 1 and table 2, and original device product fugitive constituent data from the sample survey of not using above-mentioned technology and equipment sees Table 3 and table 4.
Table 1:
| Sample number | 1 | 2 | 3 | 4 | 5 |
| Feeding rate (L/min) | 8.1 | 8.0 | 8.0 | 8.0 | 8.1 |
| One take off temperature (℃) | 121 | 118 | 138 | 140 | 142 |
| One takes off vacuum tightness (kPa) | 7.3 | 6.4 | 8.9 | 8.4 | 6.5 |
| Two take off temperature (℃) | 162 | 142 | 150 | 156 | 169 |
| Two take off vacuum tightness (kPa) | 0.8 | 1.1 | 1.5 | 0.9 | 1.5 |
| Fugitive constituent (%) | 0.030 | 0.026 | 0.031 | 0.028 | 0.027 |
Table 2:
| Sample number | 1 | 2 | 3 | 4 | 5 |
| Feeding rate (L/min) | 17.9 | 18.0 | 18.0 | 17.9 | 18.0 |
| One take off temperature (℃) | 130 | 114 | 168 | 142 | 131 |
| One takes off vacuum tightness (kPa) | 11 | 15 | 21 | 19 | 17 |
| Two take off temperature (℃) | 134 | 147 | 163 | 151 | 157 |
| Two take off vacuum tightness (kPa) | 0.8 | 0.7 | 1.6 | 0.9 | 1.5 |
| Fugitive constituent (%) | 0.021 | 0.047 | 0.039 | 0.026 | 0.042 |
Table 3 does not use processing parameter of the present invention and result with table 4 for 2kt/a o-cresol formaldehyde epoxy resin device.
Table 3:
Table 4:
| Sample number | 1 | 2 | 3 | 4 | 5 |
| Feeding rate (L/min) | 18.0 | 18.0 | 17.9 | 18.0 | 18.0 |
| One take off temperature (℃) | 141 | 147 | 160 | 157 | 123 |
| One takes off vacuum tightness (kPa) | 11 | 20 | 10 | 15 | 17 |
| Two take off temperature (℃) | 160 | 143 | 145 | 151 | 148 |
| Two take off vacuum tightness (kPa) | 0.7 | 0.6 | 0.9 | 1.4 | 0.8 |
| Fugitive constituent (%) | 0.094 | 0.093 | 0.112 | 0.099 | 0.108 |
By above list data contrast as can be known, after 2kt/a o-cresol formaldehyde epoxy resin device uses the present invention, under the condition that process conditions does not change, reached the purpose that reduces the o-cresol formaldehyde epoxy resin fugitive constituent.
Claims (10)
1. a method that reduces the o-cresol formaldehyde epoxy resin fugitive constituent is characterized in that, adopts thick desolventizing step and smart desolventizing step two-stage desolventizing step to slough solvent and high boiling material component in the o-cresol formaldehyde epoxy resin;
Described thick desolventizing step is: o-cresol formaldehyde epoxy resin solution is sent in first line mixer, pass through falling-film evaporator and gas-liquid separator again, with the solvent in the preliminary removal o-cresol formaldehyde epoxy resin solution, removed solvent is discharged from gas-liquid separator with volatile matter gas phase form, the liquid phase part of gas-liquid separator output turns back in first line mixer by reflux pump, and another part takes off extractor pump by one and enters smart desolventizing step; The solvent of being removed through thick desolventizing step accounts for more than 99% of total solvent quality;
Described smart desolventizing step is: the o-cresol formaldehyde epoxy resin solution that passes through thick desolventizing step process enters to pass through successively after the mixing in second line mixer with steam again and steams film evaporator and packing tower, take off extractor pump by two at last and discharge, in luwa evaporator and packing tower, slough remaining solvent and high boiling material composition;
Described first line mixer is the horizontal pipeline mixing tank, and described second line mixer is the riser mixing tank.
2. the method for reduction o-cresol formaldehyde epoxy resin fugitive constituent according to claim 1 is characterized in that, adopts hot nitrogen treatment technology to increase the removal efficiency of volatilizable thing in packing tower.
3. the method for reduction o-cresol formaldehyde epoxy resin fugitive constituent according to claim 1 is characterized in that, falling-film evaporator is vertical adverse current falling-film evaporator; The falling-film evaporator heating medium adopts the following low-pressure steam of 2.5MPa.
4. the method for reduction o-cresol formaldehyde epoxy resin fugitive constituent according to claim 2, it is characterized in that, luwa evaporator is vertical movable scraping plate formula vaporizer, the luwa evaporator heating medium is a thermal oil, azeotrope adopts the following low-pressure steam of 2.5MPa, and hot nitrogen temperature is controlled at 80～120 ℃.
5. the method for reduction o-cresol formaldehyde epoxy resin fugitive constituent according to claim 1 is characterized in that, in the thick desolventizing step, temperature is controlled at 90～180 ℃; The vacuum degree control of the device of thick desolventizing step correspondence is at 5～25kPa.
6. the method for reduction o-cresol formaldehyde epoxy resin fugitive constituent according to claim 1 is characterized in that, in the smart desolventizing step, the vacuum degree control of the device of smart desolventizing step correspondence is at 0.5～5kPa, and temperature is controlled at 90～180 ℃.
7. according to the method for each described reduction o-cresol formaldehyde epoxy resin fugitive constituent of claim 1-6, it is characterized in that, the filler of filling in first line mixer and second line mixer is Pall ring, Raschig ring or cascade ring, the filler mode is for huddling, the filler of filling in the packing tower is Pall ring, Raschig ring or cascade ring, the filler mode is for huddling, and the system feeding amount is for greater than 0 and be less than or equal to 20L/min.
8. device that reduces the o-cresol formaldehyde epoxy resin fugitive constituent, it is characterized in that, fresh feed pump, first line mixer, falling-film evaporator, gas-liquid separator, take off extractor pump, second line mixer, thin-film evaporator, packing tower and two and take off extractor pump and link to each other successively, some turns back to the o-cresol formaldehyde epoxy resin solution of gas-liquid separator output in first line mixer through reflux pump, in second line mixer, be provided with the steam admission port, on gas-liquid separator and thin-film evaporator, be equipped with the volatile matter gaseous phase outlet.
9. the device of reduction o-cresol formaldehyde epoxy resin fugitive constituent according to claim 8 is characterized in that, described thin-film evaporator is a luwa evaporator.
10. according to Claim 8 or the device of 9 described reduction o-cresol formaldehyde epoxy resin fugitive constituents, it is characterized in that described packing tower is provided with and is used for the inlet that hot nitrogen enters.
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| CN 201010552018 CN102464792B (en) | 2010-11-18 | 2010-11-18 | Method and device for reducing volatile matters of o-cresol-formaldehyde epoxy resin |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2017505830A (en) * | 2013-12-18 | 2017-02-23 | ブルー キューブ アイピー エルエルシー | Distilled epoxy novolac resin |
| CN105793312A (en) * | 2013-12-18 | 2016-07-20 | 蓝立方知识产权有限责任公司 | Distilled epoxy novolac resins |
| CN108654124B (en) * | 2018-05-31 | 2020-11-24 | 万华化学集团股份有限公司 | Device and method for removing volatile organic compounds in emulsion |
| CN109173318B (en) * | 2018-10-29 | 2024-06-21 | 江苏九九久科技有限公司 | Energy-saving solvent high-efficiency separation combined evaporator |
| CN111320734B (en) * | 2018-12-13 | 2022-06-24 | 航天特种材料及工艺技术研究所 | Method for reducing volatile content in resin |
| CN114681934A (en) * | 2020-12-25 | 2022-07-01 | 西安万德科技有限公司 | System for increasing concentration of mixed liquid or evaporating solvent |
| CN115068966B (en) * | 2022-08-22 | 2022-11-08 | 淄博鲁华泓锦新材料集团股份有限公司 | Continuous desolventizing and refining method for hydrogenated petroleum resin |
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| CN201873637U (en) * | 2010-11-18 | 2011-06-22 | 中国石油化工集团公司 | O-cresol-formaldehyde epoxy resin treatment device based on two-stage solvent removal agent |
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| JP2002128862A (en) * | 2000-10-27 | 2002-05-09 | Dainippon Ink & Chem Inc | Epoxy resin composition for semiconductor sealing |
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| CN201873637U (en) * | 2010-11-18 | 2011-06-22 | 中国石油化工集团公司 | O-cresol-formaldehyde epoxy resin treatment device based on two-stage solvent removal agent |
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