CN109759038A - A kind of method of silica gel after regenerative adsorption - Google Patents
A kind of method of silica gel after regenerative adsorption Download PDFInfo
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- CN109759038A CN109759038A CN201910121171.2A CN201910121171A CN109759038A CN 109759038 A CN109759038 A CN 109759038A CN 201910121171 A CN201910121171 A CN 201910121171A CN 109759038 A CN109759038 A CN 109759038A
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- silica gel
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Abstract
The present invention relates to a kind of methods of silica gel after regenerative adsorption, comprising the following steps: silica gel after absorption and mixed solvent are mixed in a certain ratio stirring, and control whipping temp and mixing time；Settle and separate；It silica gel containing solvent and is separately handled containing oil solvent after separation, solvent-laden silica gel is by the isolated rebirth silica gel of method of distillation, and desolventizing after first separating containing oil solvent, solvent and rebirth silica gel are recycled.The present invention recycles cycling and reutilization silica gel under the premise of economic and environment-friendly, silica gel can Infinite Cyclic use, and loss amount is small；Compared with silica gel method after calcination method recycling absorption, the oil being adsorbed in silica gel can be not only recycled, but also silica gel loss amount is small, and not will cause environmental pollution.
Description
Technical field
The invention belongs to silica regeneration technical fields, and in particular to a kind of method of silica gel after regenerative adsorption.
Background technique
Silica gel as adsorbent it is a kind of in petrochemical industry production by the general application of wide, become useless after silica gel absorption saturation
Silica gel, poisonous and harmful, how to handle useless silica gel becomes the problem of many enterprises.Some enterprises are using the method processing directly burned
Useless silica gel was also met useless with the processing of rotary kiln furnace because silica gel has a large amount of combustible oily substances in petrochemical industry production
The report of silica gel, through rotary kiln furnace, treated that silica gel is also reusable, realizes the regeneration of silica gel.But no matter directly burn also
Be: the processing of rotary kiln furnace is operated first that process is all unfriendly to site environment, and the oily useless silica gel of band takes out from adsorption tower, then
It is sent into furnace or rotary kiln furnace, operating process will cause pollution, minimum air pollution is difficult to eliminate；Secondly uneconomical, because of silica gel
The oily substance and silica gel quality of absorption are than substantially 1:1, this part oil product is wasted after burning；It is not square that there are also operations
Just, silica gel is taken out and is loaded repeatedly.Therefore, the silica gel after absorption can be carried out again by designing one kind (such as the silica gel after adsorbing)
It gives birth to, reduce environmental pollution, the operating method for the utilization rate for improving silica gel has important economy, society, the value of environmental protection and reality
Meaning.
Summary of the invention
The object of the invention is that solve the above-mentioned problems and to provide a kind of structure simple, design it is reasonable it is a kind of again
The method of silica gel after raw absorption.
The present invention through the following technical solutions to achieve the above objectives:
A kind of method of silica gel after regenerative adsorption, comprising the following steps:
S1: taking useless silica gel and solvent in proportion, stirs, and is uniformly mixed；
S2: standing, and isolates solvent-laden silica gel and containing oil solvent；
S3: separating treatment is carried out to silica gel containing solvent obtained in step S2, obtains rebirth silica gel and solvent after dry；
S4: separating treatment is carried out to oil solvent is contained obtained in step S2, obtains solvent and oil.
As a further optimization solution of the present invention, solvent is NMP and diethanol amine mixed solvent in the step S1, two
The mixed proportion of person is 1:0.05.
As a further optimization solution of the present invention, the mixed proportion of useless silica gel and solvent is 2-1:1 in the step S1.
As a further optimization solution of the present invention, time of repose is 1-2min in the step S2, and mixing time is
0.5-1h, whipping temp are 60-70 DEG C.
As a further optimization solution of the present invention, the solvent method that goes of the silica gel containing solvent is that decompression is steamed in the step S3
Evaporate separation method.
As a further optimization solution of the present invention, the separation method containing oil solvent is a negative atmosphere in the step S4
It presses, be evaporated under reduced pressure under the conditions of 160 DEG C.
As a further optimization solution of the present invention, the solvent separated in the step S3 is transferred to step S1 recycling.
As a further optimization solution of the present invention, the solvent separated in the step S4, which is transferred in S1, to be recycled.
The beneficial effects of the present invention are:
1) present invention under the premise of economic and environment-friendly, recycle cycling and reutilization silica gel, silica gel can Infinite Cyclic use, and damage
Vector is small；
2) present invention can not only be recycled and be adsorbed in silica gel compared with silica gel method after calcination method recycling absorption
Oil, and silica gel loss amount is small, and not will cause environmental pollution；
3) knot method of the present invention is simple, and stability is high, and design rationally, is easy to implement.
Specific embodiment
The application is described in further detail below, it is necessary to which indicated herein to be, following specific embodiments are only used
It is further detailed in the application, should not be understood as the limitation to the application protection scope, person skilled in art
Some nonessential modifications and adaptations can be made to the application according to above-mentioned application content.
A kind of method of silica gel after regenerative adsorption, comprising the following steps:
S1: being the NMP of 1:0.05 and the mixed solution of diethanol amine as solvent using volume ratio, 2-1:1 in mass ratio takes useless
Silica gel and the solvent are uniformly mixed, and at 60-70 DEG C, stir 0.5-1h；
S2: being stored at room temperature 1-2min for mixture in step S1, isolates silica gel containing solvent and containing oil solvent；
S3: with a negative atmospheric pressure, the vacuum distillation of 160 DEG C of conditions method to silica gel containing solvent obtained in step S2 into
Row separating treatment, obtains rebirth silica gel and solvent；
S4: it is carried out to obtained in step S2 containing oil solvent in the method for a negative atmospheric pressure, 160 DEG C of condition vacuum distillations
Separating treatment obtains solvent and oil.
It should be noted that the solvent obtained in the step S3 is transferred to step S1 recycling, divide in the step S4
From solvent be transferred in S1 and be recycled.
Embodiment 1
A kind of method of silica gel after regenerative adsorption, comprising the following steps:
S1: using volume ratio for 1:0.05 NMP and diethanol amine mixed solution as solvent, 2:1 in mass ratio takes useless silica gel
It with the solvent, is uniformly mixed, at 60 DEG C, stirs 1h, wherein useless silica gel is 10000g；
S2: being stored at room temperature 2min for mixture in step S1, isolates silica gel containing solvent and containing oil solvent；
S3: with a negative atmospheric pressure, the vacuum distillation of 160 DEG C of conditions method to silica gel containing solvent obtained in step S2 into
Row separating treatment, obtains rebirth silica gel and solvent；
S4: it is carried out to obtained in step S2 containing oil solvent in the method for a negative atmospheric pressure, 160 DEG C of condition vacuum distillations
Separating treatment obtains solvent and oil.
Embodiment 2
A kind of method of silica gel after regenerative adsorption, comprising the following steps:
S1: using volume ratio for 1:0.05 NMP and diethanol amine mixed solution as solvent, 1:1 in mass ratio takes useless silica gel
It with the solvent, is uniformly mixed, at 65 DEG C, stirs 45min, wherein useless silica gel is 10000g；
S2: being stored at room temperature 1.5min for mixture in step S1, isolates silica gel containing solvent and containing oil solvent；
S3: with a negative atmospheric pressure, the vacuum distillation of 160 DEG C of conditions method to silica gel containing solvent obtained in step S2 into
Row separating treatment, obtains rebirth silica gel and solvent；
S4: it is carried out to obtained in step S2 containing oil solvent in the method for a negative atmospheric pressure, 160 DEG C of condition vacuum distillations
Separating treatment obtains solvent and oil.
Embodiment 3
A kind of method of silica gel after regenerative adsorption, comprising the following steps:
S1: using volume ratio for 1:0.05 NMP and diethanol amine mixed solution as solvent, 1.5:1 in mass ratio takes useless silicon
Glue and the solvent are uniformly mixed, and at 70 DEG C, stir 30min, wherein useless silica gel is 10000g；
S2: being stored at room temperature 1min for mixture in step S1, isolates silica gel containing solvent and containing oil solvent；
S3: with a negative atmospheric pressure, the vacuum distillation of 160 DEG C of conditions method to silica gel containing solvent obtained in step S2 into
Row separating treatment, obtains rebirth silica gel and solvent；
S4: it is carried out to obtained in step S2 containing oil solvent in the method for a negative atmospheric pressure, 160 DEG C of condition vacuum distillations
Separating treatment obtains solvent and oil.
Embodiment 4
A kind of method of silica gel after regenerative adsorption, comprising the following steps:
S1: using volume ratio for 1:0.05 NMP as solvent, 2:1 in mass ratio takes useless silica gel and the solvent, and mixing is equal
It is even, at 60 DEG C, 1h is stirred, wherein useless silica gel is 10000g；
S2: being stored at room temperature 2min for mixture in step S1, isolates silica gel containing solvent and containing oil solvent；
S3: with a negative atmospheric pressure, the vacuum distillation of 160 DEG C of conditions method to silica gel containing solvent obtained in step S2 into
Row separating treatment, obtains rebirth silica gel and solvent；
S4: it is carried out to obtained in step S2 containing oil solvent in the method for a negative atmospheric pressure, 160 DEG C of condition vacuum distillations
Separating treatment obtains solvent and oil.
Embodiment 5
A kind of method of silica gel after regenerative adsorption, comprising the following steps:
S1: using volume ratio for 1:0.05 diethanol amine as solvent, 2:1 in mass ratio takes useless silica gel and the solvent, mix
It closes uniformly, at 60 DEG C, stirs 1h, wherein useless silica gel is 10000g；
S2: being stored at room temperature 2min for mixture in step S1, isolates silica gel containing solvent and containing oil solvent；
S3: with a negative atmospheric pressure, the vacuum distillation of 160 DEG C of conditions method to silica gel containing solvent obtained in step S2 into
Row separating treatment, obtains rebirth silica gel and solvent；
S4: it is carried out to obtained in step S2 containing oil solvent in the method for a negative atmospheric pressure, 160 DEG C of condition vacuum distillations
Separating treatment obtains solvent and oil
Embodiment 6
It is known that the absorption oil total amount of silica gel are as follows: silica gel calcining front and back is of poor quality after absorption；Silica gel de-oiling amount after absorption
Are as follows: the oily total amount isolated after silica gel de-oiling operation after absorption；Therefore, η1(silica gel de-oiling ratio after absorption)=(silicon after absorption
Glue de-oiling amount)/(the absorption oil total amount of silica gel) * 100%=M1(the oily total amount isolated after silica gel de-oiling operation after absorption)/N1
(silica gel calcining front and back is of poor quality after absorption) * 100%.
Similarly, η2(the loss ratio of silica gel)=M2(silica gel total amount after silica gel de-oiling after absorption)/N2(silica gel is total after absorption
Amount) * 100%；
η3(NMP loses ratio)=M3(the NMP total amount isolated after silica gel de-oiling after absorption)/N3(silica gel de-oiling after absorption
Operate NMP otal investment) * 100%.
According to relation above formula, the de-oiling amount obtained in above-described embodiment, silica gel loss amount and NMP loss amount are carried out pair
Than, and relative percentage is calculated, result such as following table 1-3:
Silica gel de-oiling ratio compares after table 1 adsorbs
| M1(g) | N1(g) | η1(%) | |
| Embodiment 1 | 494.3 | 502.4 | 98.4 |
| Embodiment 2 | 491.8 | 502.4 | 97.9 |
| Embodiment 3 | 492.8 | 502.4 | 98.1 |
| Embodiment 4 | 478.8 | 502.4 | 95.3 |
| Embodiment 5 | 484.8 | 502.4 | 96.5 |
Table 1 the result shows that: using solvent refining method to after absorption silica gel carry out deoiling treatment method, de-oiling
Ratio is relatively high, and maximum de-oiling ratio is 98.4%, and de-oiling ratio is high, and effect is obvious, with single solvent to silica gel after absorption
The comparison of de-oiling ratio, mixed solvent becomes apparent the de-oiling effect of silica gel after absorption.
The loss ratio of 2 silica gel of table compares
| M2(g) | N2(g) | η2 | |
| Embodiment 1 | 0.995 | 497.6 | 0.2 |
| Embodiment 2 | 0.846 | 497.6 | 0.17 |
| Embodiment 3 | 0.796 | 497.6 | 0.16 |
| Embodiment 4 | 1.99 | 497.6 | 0.4 |
| Embodiment 5 | 2.29 | 497.6 | 0.46 |
Table 2 the result shows that: using mixed solvent to after absorption silica gel carry out deoiling treatment method compared to single
For solvent TOEFL silica gel, the loss late of silica gel is lower, and effect is more preferable, and regeneration efficiency is high.
3 NMP of table loses ratio comparison
| M3(g) | N3(g) | η3 | |
| Embodiment 1 | 1.2 | 1000 | 0.12 |
| Embodiment 2 | 1.5 | 1000 | 0.15 |
| Embodiment 3 | 1.3 | 1000 | 0.13 |
| Embodiment 4 | 2.1 | 1000 | 0.21 |
| Embodiment 5 | 2.3 | 1000 | 0.23 |
Table 3 the result shows that: single solvent and mixed solvent carry out deoiling treatment to silica gel after absorption, for nmp solvent
When being recycled, for the yield of the NMP recycled from each method and the loss late of NMP, the NMP of in the mixed solvent can be obtained
To maximum utilize, and loss amount compare it is lower for single solvent.
Embodiment 7
The adsorption capacity comparative experiments of rebirth silica gel and new silica gel is as follows after desorption:
The rebirth silica gel 10000g for taking new silica gel and above-described embodiment to obtain, respectively adsorbs the base oil of isodose
Extraction procedure, the quality of the silica gel after being adsorbed and unadsorbed silica gel quality are as follows
Table 4:
Upper table the result shows that: the silica gel of mixed solvent method desorption and regeneration its to the absorption of base oil extracting performance and new silica gel
Very close to can normal use.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.
Claims (7)
1. a kind of method of silica gel after regenerative adsorption, which comprises the following steps:
S1: taking useless silica gel and solvent in proportion, stirs, and is uniformly mixed；
S2: standing, and isolates solvent-laden silica gel and containing oil solvent；
S3: separating treatment is carried out to silica gel containing solvent obtained in step S2, obtains rebirth silica gel and solvent after dry；
S4: separating treatment is carried out containing oil solvent to what is separated in step S2, obtains solvent and oil.
2. the method for silica gel after a kind of regenerative adsorption according to claim 1, it is characterised in that: solvent in the step S1
For NMP and diethanol amine mixed solvent, the mixed proportion of the two is 1:0.05.
3. the method for silica gel after a kind of regenerative adsorption according to claim 1, it is characterised in that: give up silicon in the step S1
The mixed proportion of glue and solvent is 2-1:1.
4. the method for silica gel after a kind of regenerative adsorption according to claim 1, it is characterised in that: stood in the step S2
Time is 1-2min, and mixing time 0.5-1h, whipping temp is 60-70 DEG C.
5. the method for silica gel after a kind of regenerative adsorption according to claim 1, it is characterised in that: containing molten in the step S3
Agent silica gel goes solvent method for vacuum distillation separation method.
6. the method for silica gel after a kind of regenerative adsorption according to claim 1, it is characterised in that: oil-containing in the step S4
The separation method of solvent is a negative atmospheric pressure, is evaporated under reduced pressure under the conditions of 160 DEG C.
7. the method for silica gel after a kind of regenerative adsorption according to claim 1, it is characterised in that: separated in the step S3
Solvent be transferred to step S1 recycling.
The method of silica gel after a kind of regenerative adsorption according to claim 1, it is characterised in that: separated in the step S4
Solvent is transferred in S1 and is recycled.
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| CN109701507A (en) * | 2019-01-25 | 2019-05-03 | 安徽国孚凤凰科技有限公司 | A kind of the solvent desorbing device and process of silica gel purification Reclaimed Base Oil |
| CN111944597A (en) * | 2020-07-20 | 2020-11-17 | 安徽国孚润滑油工业有限公司 | Dissolved residual oil adsorption process by using primary waste silicone oil glue |
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