CN101235105A - Method for agglomerating solution-polymerized rubber - Google Patents
Method for agglomerating solution-polymerized rubber Download PDFInfo
- Publication number
- CN101235105A CN101235105A CNA2007101593540A CN200710159354A CN101235105A CN 101235105 A CN101235105 A CN 101235105A CN A2007101593540 A CNA2007101593540 A CN A2007101593540A CN 200710159354 A CN200710159354 A CN 200710159354A CN 101235105 A CN101235105 A CN 101235105A
- Authority
- CN
- China
- Prior art keywords
- glue
- cohesion
- still
- water
- aggregation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Adhesives Or Adhesive Processes (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention relates to a solution polymerization rubber aggregation method, which comprises using steam as energy and overheat water as separation medium, completely mixing rubber liquid and overheat water, increasing temperature, evaporating most solvents at the instant of ejecting rubber solution-hot water into the hot water in aggregation pot to complete the pre-aggregation of rubber solution and reduce the solvent consumption in aggregation. The invention is suitable for aggregation in polybutadiene rubber production and suitable for the aggregation in solution polymerization rubber liquid sedimentation method to complete separation of polymer and solvent synchronous via flash evaporation and sedimentation methods, thereby resolving the contradictory between aggregation energy consumption and material consumption in sedimentation method. The invention uses pre-aggregation technique in sedimentation method to reduce solvent consumption without additional energy consumption, thereby resolving the contradictory between aggregation energy consumption and material consumption in sedimentation to optimiz aggregation processing parameters and realize energy saving and discharge reduction.
Description
Technical field
The invention belongs to separation method, particularly relate to a kind of method for agglomerating solution-polymerized rubber.
Background technology
Except containing polyhutadiene, still contain solvent and unreacted divinyl in the cis-1,4-polybutadiene rubber polymerization glue, must just can obtain the cis-1,4-polybutadiene rubber product through cohesion, drying.At nickel is in the butadiene solution polymerization process, end still temperature of reaction generally is controlled at about 95 ℃, butadiene conversion can reach about 85%, and for energy consumption and the material consumption that reduces agglomeration process, domestic cis-1,4-polybutadiene rubber production equipment has generally adopted insulation measure and glue flash evaporation technology to the glue jar.After glue entered the glue jar, most of unreacted divinyl was flashed from tank deck and discharges and reclaim, and the glue that removes to condense still can be regarded the homogeneous phase solution of polyhutadiene and solvent as, and therefore, agglomeration process can be considered the technological process that solvent is deviate from.
Cis-1,4-polybutadiene rubber production energy consumption (steam consumption) mainly occurs in the glue agglomeration process with material consumption (solvent consumption), and cohesion solvent consumption major part directly enters atmosphere at after-treatment system.Therefore, cohesion energy consumption and material consumption are the important symbols of cohesion production technology level, it not only is related to the economic benefit that cis-1,4-polybutadiene rubber is produced, and is related to environmental issue, makes the energy-saving and cost-reducing research of cohesion become the important subject of cis-1,4-polybutadiene rubber production energy-saving and emission-reduction.
Since the cis-1,4-polybutadiene rubber industrialization, adopted elutriation method isolating polymer and solvent both at home and abroad always, be about to glue and spray in the cohesion still hot water, with steam with the solvent vaporization and take out of outside the still.China's cis-1,4-polybutadiene rubber is produced the initial stage, in order to ensure the cohesion of certain throughput and glue fully, adopts higher condensation temperature and lower working pressure, and steam consumption quantity reaches more than the 10t/t glue, and the energy consumption height becomes the principal contradiction of agglomeration process.
Practice and cohesion Energy saving theory studies have shown that condensation temperature is certain, and steam consumption quantity descends with the raising of working pressure.In order to reduce steam consumption, in two still agglomeration processes, all keep certain working pressure to be called the pressurize cohesion No. 1 still, No. 2 stills, claim isobaric cohesion again.Adopt isobaric cohesion, along with the raising of working pressure, energy consumption descends, and material consumption is risen, and makes the particularly thorny of energy consumption and material consumption, has produced the differential pressure condensation technique.
In two still cohesion process, about 95% solvent is steamed by No. 1 still, and the steam consumption major part is at No. 1 still, therefore.No. 1 still adopts higher working pressure, focuses on energy-conservation; No. 2 still behaviour adopts lower working pressure, focuses on consumption reduction, is called the differential pressure cohesion.Employing differential pressure cohesion, No. 2 stills no longer only are the continuation that steam of No. 1 still solvent and replenish, and have alleviated contradiction energy-conservation and consumption reduction.
The energy-saving and cost-reducing theoretical investigation of elutriation method cohesion proves that the required sensible heat of agglomeration process solvent, latent heat steam consumption quantity xanthan are less than one ton, and it is little influenced by operational condition, can regard certain value as, and energy-conservation key is to reduce the steam consumption quantity of taking vapor phase solvent from the cohesion still out of; At the elutriation method agglomeration process, solvent vaporization impellent height, material consumption is low, the energy consumption height, solvent vaporization impellent is low, the material consumption height, energy consumption is low, and solvent vaporization impellent is the sign of material consumption, it is again the tie that connects energy consumption and material consumption, cohesion energy consumption and material consumption are to be a pair of contradiction of tie with the solvent impellent of vaporizing, and they condition each other, and must take into account again; Pass through Theoretical Calculation, can draw out the vaporization of solvent under different operating condition impellent and see Fig. 1 with the relation curve of taking the vapor phase solvent steam consumption quantity from the cohesion still out of, on behalf of solvent vaporization impellent (MPa), Y, X represent steam consumption quantity t/t glue, among the figure condensation temperature of curve: 1-92 ℃; 2-94 ℃; 3-96 ℃; 4-98 ℃; 5-100 ℃; 6-102 ℃.It has disclosed the relation of condensation temperature, working pressure and energy consumption, material consumption, becomes the reliable basis of selecting and optimizing the cohesion process condition.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art, has worked out a kind ofly under the condition that does not increase energy consumption, reduces material consumption, improves the effect and the alkali cleaning effect of dispersion agent; On the basis that reduces material consumption, optimize the cohesion process condition, further energy-conservation method for agglomerating solution-polymerized rubber.
Method for agglomerating solution-polymerized rubber of the present invention, be before the glue cohesion, increase pre-cohesion process process,, do medium with superheated water to make the energy with steam, allow glue and superheated water thorough mixing also heat up, enter the moment of condensing still hot water at glue-hot water, most of solvent is flashed vaporization, reduces solvent consumption on the basis that does not increase energy consumption, on the basis of consumption reduction, optimize cohesion process condition and further energy-conservation, dissolve the method for agglomeration process energy consumption and material consumption contradiction.Concrete summary of the invention is as follows:
A, heat water to 115 ℃～130 ℃ and make superheated water, and add polycarboxylic acid sodium dispersion agent and sodium hydroxide lye, the dispersion agent add-on is 1 * 10 of a dry glue quality
-4～5 * 10
-4, alkali lye add-on to the pH value of control cohesion hot water is between 9～10;
B, with the superheated water solution thorough mixing that glue and a step make, obtain the non-homogeneous mixture of 113 ℃～125 ℃ of glue-hot water;
C, glue-hot water non-homogeneous mixture sprayed be injected with in the cohesion still of 93 ℃～100 ℃ of hot water, promptly finished the pre-agglomeration process of glue;
The control residence time was 40～50 minutes under glue after d, the pre-cohesion continued to stir in the cohesion still, promptly finished the elutriation method agglomeration process.
As a further improvement on the present invention, the mixed volume ratio of glue and superheated water is 1: 2～3 in the b step.
As a further improvement on the present invention, the spraying pressure in the c step is 0.4MPa～0.8MPa.
Pre-condensation principle: change the adding mode of part cohesion with steam, with glue and the superheated water thorough mixing that adds dispersion agent and alkali lye, allow the enough solvent vaporization potential of glue-hot water storage, spray into moment in the cohesion hot water at glue-hot water, most of solvent is depressurized flash distillation, rapidly vaporization.
Agglomerating solution-polymerized rubber device of the present invention is to be made of steam heater, glue mixing tank, pre-lime set nozzle and cohesion still.The outlet line of steam heater is connected with glue mixing tank pipeline, and the outlet of glue mixing tank connects pre-lime set nozzle, and the outlet of pre-lime set nozzle places 1
#In the cohesion still, 1
#The outlet line of cohesion still is through pump and 2
#The cohesion still connects.Wherein, dispersion agent inlet c, alkali liquor inlet d and glue inlet e are arranged having on the steam heater on recirculated water inlet a and steam-in b, its outlet line; 1
#Recirculated water inlet f and steam-in g are arranged on the cohesion still; 2
#Steam-in i, gas phase precipitate outlet j and micelle water out k are arranged on the cohesion still.Steam heater is steam to be mixed with circulating hot water produce superheated water; The glue mixing tank is with glue and superheated water thorough mixing, obtains pyritous glue-hot water non-homogeneous mixture, and the glue mixing tank is a static mixer, and static mixer must be able to allow glue and superheated water thorough mixing; Pre-lime set nozzle is to condense in the hot water except glue-hot water is sprayed into, and another vital role of pre-lime set nozzle is to have pressure holding function, does not vaporize to ensure pre-condensed system superheated water and solvent.
Pre-cohesion process design considerations and processing condition are selected:
At pre-agglomeration process, solvent and aqueous nature difference are very big, can regard two systems that are independent of each other as; Not to be polyhutadiene be scattered in glue in the solvent with molecularity for polyhutadiene and solvent, and the molecular weight of polyhutadiene and the molecular weight of solvent differ greatly, its molar fraction is again little, the flash of steam of solvent can be ignored by the influence of polyhutadiene, therefore, to pre-agglomeration process, can determine superheated water minimum permissible temperature and corresponding pre-condensation temperature by solvent adiabatic flash heat balance.
At pre-agglomeration process, glue-hot water temperature is that pre-condensation temperature is the key of the pre-flocculating result of influence, the effect of steam is to realize by the thorough mixing of glue and superheated water, therefore, from being designed into production all with the sign of superheated water temperature as pre-condensation temperature, the superheated water temperature becomes the important process control condition of pre-agglomeration process.Be example with the pre-agglomeration process of cis-1,4-polybutadiene rubber below, its superheated water minimum permissible temperature and corresponding pre-condensation temperature are calculated.
1. superheated water minimum permissible temperature
To produce an xanthan, calculate the superheated water minimum permissible temperature that can satisfy the required energy of pre-cohesion glue.Make following setting according to production practice.
Set: the about 8.5m of glue volume that produces an xanthan
3
Produce in the glue of an xanthan and contain 4.5 tons of solvents;
1# still solvent vaporization rate is 95%;
Glue temperature is 85 ℃;
Condensation temperature is 96 ℃～98 ℃;
Pre-cohesion water/glue 2～3;
Solvent is in hexane.
Other relevant physico-chemical constants see Table 1.
The relevant physico-chemical constant of table 1 agglomeration process
| Meaning | Unit | Numerical value |
| The hexane thermal capacitance | kJ/(kg·℃) | 2.27 |
| The cis-1,4-polybutadiene rubber thermal capacitance | kJ/(kg·℃) | 2.09 |
| The thermal capacitance of water | kJ/(kg·℃) | 4.19 |
| The hexane enthalpy of vaporization | kJ/kg | 3.36×10 2 |
A. sensible heat
At pre-agglomeration process, the heating glue is to the needed sensible heat Q of condensation temperature
1For:
Q
1＝(C
1×m
1+C
2×m
2)×(t
3-t
4) (1)
C in the formula
1The thermal capacitance of-solvent, kJ/ (kg ℃);
C
2The thermal capacitance of-cis-1,4-polybutadiene rubber, kJ/ (kg ℃);
m
1The quality of solvent in the glue of-product 1 xanthan, kg;
m
2-cis-1,4-polybutadiene rubber output, 1000kg;
t
3-condensation temperature, ℃;
t
4-glue temperature, ℃.
B. latent heat
At pre-agglomeration process, the latent heat Q that the vaporization of 95% solvent needs in the glue
3For:
Q
2＝ΔH
1×m
1×95％ (2)
Δ H in the formula
1The enthalpy of vaporization of-solvent, kJ/ (kg ℃).
C. superheated water minimum permissible temperature
At pre-agglomeration process, superheated water is reduced to the heat balance equation of condensation temperature liberated heat and the required sensible heat of glue, latent heat:
Q
1+Q
2＝C
3×8.5×1000×R×(t
5-t
3) (3)
C in the formula
3The thermal capacitance of-water, kJ/ (kg ℃);
8.5-produce the glue volume of 1 xanthan, m
3
R-condenses water/glue in advance;
t
5-superheated water temperature, ℃.
With (1), (2) formula substitution (3) formula through abbreviation, then:
Condensation temperature is 98 ℃, calculates the superheated water minimum permissible temperature by (4) formula:
When R=2, t
5=120.4 (℃);
When R=2.5, t
5=115.9 (℃);
When R=3, t
5=112.9 (℃).
Condensation temperature is 96 ℃, calculates the superheated water minimum permissible temperature by (4) formula:
When R=2, t
5=118.1 (℃);
When R=2.5, t
5=113.7 (℃);
When R=3, t
5=110.8 (℃).
2. superheated water temperature and condensation temperature in advance
At pre-agglomeration process, the heat balance equation that superheated water heat release and glue heat up:
(C
1×m
1+C
2×m
2)×(t
6-t
4)＝C
3×8.5×1000×R×(t
5-t
6) (5)
T in the formula
6-pre-condensation temperature, ℃.
With (4) formula substitution (5) formula through abbreviation, then:
Condensation temperature is 98 ℃, is calculated and the corresponding pre-condensation temperature of superheated water minimum permissible temperature by (6) formula:
When R=2, t
6=114.0 (℃);
When R=2.5, t
6=111.2 (℃);
When R=3, t
6=109.2 (℃).
Condensation temperature is 96 ℃, is calculated and the corresponding pre-condensation temperature of superheated water minimum permissible temperature by (6) formula:
When R=2, t
6=113.2 (℃);
When R=2.5, t
6=110.2 (℃);
When R=3, t
6=108.1 (℃).
3. the superheated water temperature is selected
At pre-agglomeration process, it is relevant with condensation temperature and pre-cohesion water/glue that the superheated water temperature is selected.Solvent adiabatic flash process of hot potassium heat balance is combined with production practice, draw out pre-cohesion water/glue and superheated water minimum permissible temperature and corresponding pre-condensation temperature relation curve under the different condensation temperatures, see Fig. 2, X represents pre-coagel/water, the Y representation temperature (℃), it is for determining pre-cohesion process design conditions and selecting pre-cohesion process condition that foundation is provided:
Curve among Fig. 2: when 1, on behalf of condensation temperature, 2-be 98 ℃, superheated water minimum permissible temperature and corresponding pre-condensation temperature; When 3, on behalf of condensation temperature, 4-be 96 ℃, superheated water minimum permissible temperature and corresponding pre-condensation temperature.
As seen from Figure 2, No. 1 still condensation temperature is at 96 ℃～98 ℃, condenses water/glue 〉=2 o'clock in advance, and the superheated water temperature is controlled at 120 ℃～125 ℃, it carries heat energy not only will heat glue to condensation temperature, and can satisfy the enough solvent vaporization potential of pre-agglomeration process glue-hot water storage.Therefore, No. 1 still condensation temperature condenses water/glue in advance and is controlled at 2.5 ± 0.5 at 97 ± 1 ℃, and the superheated water temperature is advisable with 120 ℃～125 ℃.
Therefore, adopt pre-condensation technique of the present invention can optimize the cohesion process condition, the cohesion process condition after the optimization is: 1
#Cohesion still temperature is controlled at 93 ℃～99 ℃, and pressure-controlling is at 0.06MPa～0.10MPa; 2
#Cohesion still temperature is controlled at 96 ℃～102 ℃, and pressure-controlling is at 0.02MPa～0.04MPa.
Method for agglomerating solution-polymerized rubber of the present invention is used at the cis-1,4-polybutadiene rubber agglomeration process, receives effect preferably:
1., in the condition that does not increase energy consumption, reduce more than the solvent consumption 10kg/t glue, adopt pre-condensation technique before, this part solvent all enters atmosphere by after-treatment system;
2., containing quantity of solvent in good, the glue of cohesion micelle drying property reduces;
3., alleviated the corrosion of cohesion and finishing apparatus, pipeline;
4., on the basis of consumption reduction, optimize the cohesion process condition, further energy-conservation.
Great effect of the present invention is, its not only is suitable for cis-1,4-polybutadiene rubber agglomeration process, and generally is applicable to and contains intermingle with glue elutriation method agglomeration process, and polymkeric substance and separating by flash method and two kinds of methods of elutriation method of solvent are finished jointly; Adopting pre-condensation technique is the reliable approach that reduces solvent consumption under the condition that does not increase energy consumption, dissolved the contradiction of elutriation method cohesion energy consumption and material consumption, basic enterprising one-step optimization cohesion process condition at consumption reduction, reach the purpose of energy-saving and emission-reduction, and alleviated equipment corrosion, eliminate potential safety hazard, improved quality product.
Description of drawings
Fig. 1 is a solvent vaporization impellent and the xanthan steam consumption quantity curve of taking vapor phase solvent out of under the different operating condition.
Fig. 2 is pre-cohesion water/glue and superheated water minimum permissible temperature and a corresponding pre-condensation temperature relation curve under the different condensation temperatures.
Fig. 3 is the structural representation of agglomerating solution-polymerized rubber device of the present invention.
Embodiment
Condense embodiment in advance below in conjunction with cis-butadiene cement liquid and further specify the present invention, but do not limit the scope of the invention.Described in an embodiment 1
#Still promptly is a cohesion still 4,2
#Still promptly is a cohesion still 5, and working pressure is a gauge pressure, solvent evaluation glue flocculating result in solvent and the micelle in No. 1 vibratory screening apparatus micelle of employing aftertreatment size, the emission gases.
By cohesion water: glue is 4.5: 1, with circulating hot-water pump by water: glue is circulating hot water to be squeezed into steam heater in 3: 1, and rest part is by the top adding of cohesion still;
In steam heater, pre-condensed system circulating hot water is heated to 120 ℃ with steam;
By dispersion agent/dried glue is 0.03% dispersion agent to be added in the superheated water;
By condensation heat water ph value 9.0～10.0 scopes that are controlled at alkali lye is added in the superheated water;
Press 30m
3/ h flow is squeezed into the glue mixing tank with glue, with the superheated water thorough mixing, sprays into through pre-lime set nozzle in the hot water of 98 ℃ of cohesion stills in the glue mixing tank, and lime set nozzle spray spraying pressure is 0.4MPa～0.8MPa.
Controlling No. 1 still condensation temperature and be 99 ℃, working pressure is 0.04MPa;
Controlling No. 2 still condensation temperatures and be 101 ℃, working pressure is 0.035MPa.
Experimental result sees Table 1.
The superheated water temperature is 115 ℃, and other experiment conditions are with embodiment 1, and experimental result sees Table 1.
Comparative Examples 1
By water: glue is circulating hot water to be squeezed into pre-lime set nozzle in 5: 1;
By dispersion agent/dried glue is 0.05% dispersion agent to be added in the cohesion still;
Pressing condensation heat water ph value control 9.0～10.0 scopes adds alkali lye in the cohesion still;
Press 28m
3/ h flow is squeezed into pre-lime set nozzle with glue, mixes with circulating hot water to spray into the cohesion still;
Other experiment conditions are with embodiment 1, and experimental result is shown in Table 1.
Table 1 different technology conditions is to the influence of flocculating result
| Project | Colloid diameter/ |
1
#Contain solvent/% in the vibratory |
1 #Vibratory screening apparatus discharging gas contains solvent/g/m 3 |
| Embodiment 1 | 2～4 | 0.33 | 13.27 |
| |
3～5 | 0.46 | 16.18 |
| Comparative Examples 1 | 4～10 | 1.07 | 30.10 |
The superheated water temperature is 127 ℃; No. 1 still condensation temperature is that 96 ℃, working pressure are 0.09MPa; No. 2 still condensation temperatures are that 99 ℃, working pressure are outside the 0.04MPa, and other experiment conditions are with embodiment 1, and experimental result sees Table 2.
The superheated water temperature is 125 ℃; No. 1 still temperature condensation degree is that 97 ℃, working pressure are 0.09MPa; No. 2 the still condensation temperature is 99 ℃, and other experiment conditions are with embodiment 1, and experimental result sees Table 2.
The superheated water temperature is 120 ℃; No. 1 still condensation temperature is that 98 ℃, working pressure are 0.08MPa; No. 2 the still condensation temperature is 100 ℃, and other experiment conditions are with embodiment 1, and experimental result sees Table 2.
The superheated water temperature is 118 ℃; No. 1 still condensation temperature is that 99 ℃, working pressure are 0.07MPa; No. 2 still condensation temperatures are that 100 ℃, working pressure are 0.03MPa, and other experiment conditions are with embodiment 1, and experimental result sees Table 2.
115 ℃, No. 1 cohesion still working pressure of superheated water temperature is that 0.06MPa, temperature are that 99 ℃, No. 2 still condensation temperatures are that 101 ℃, No. 2 still working pressures are outside the 0.03MPa, and other experiment conditions are with embodiment 1, and experimental result sees Table 2.
Comparative Examples 2
Cohesion still working pressure is the 0.08MPa except that No. 1, and other experiment conditions are with Comparative Examples 1, and experimental result sees Table 2.
Table 2 different condition is to the influence of flocculating result
| Project | Colloid diameter/ |
1
#Contain solvent/% in the vibratory |
1 #Vibratory screening apparatus discharging gas contains solvent/g/m 3 |
| Embodiment 3 | 2～4 | 0.38 | 14.27 |
| |
2～4 | 0.42 | 15.18 |
| |
2～4 | 0.37 | 15.27 |
| |
2～4 | 0.39 | 16.10 |
| |
3～5 | 0.47 | 18.16 |
| Comparative Examples 2 | 4～18 | 1.39 | 46.26 |
As can be seen from the above Examples and Comparative Examples, adopt the inventive method,, all can reduce to condense the granularity of micelle, improve the vaporization rate of solvent, reduce solvent consumption no matter be at isobaric agglomeration process or differential pressure agglomeration process; Simultaneously as can be seen, adopt the inventive method, improve the superheated water temperature, can reduce condensation temperature or/and improve the cohesion working pressure, further energy-conservation on the basis of consumption reduction, can reach energy-saving and emission-reduction purpose of the present invention fully.
Method for agglomerating solution-polymerized rubber of the present invention, realize through following steps:
A, heat water to 115 ℃～130 ℃ and make superheated water, and add polycarboxylic acid sodium dispersion agent and sodium hydroxide lye, the dispersion agent add-on is 1 * 10 of a dry glue quality
-4～5 * 10
-4, alkali lye add-on to the pH value of control cohesion hot water is between 9～10;
B, with the superheated water solution thorough mixing that glue and a step make, obtain the non-homogeneous mixture of 113 ℃～125 ℃ of glue-hot water; Glue is 1: 2～3 with the mixed volume ratio of superheated water;
C, glue-hot water non-homogeneous mixture sprayed be injected with in the cohesion still of 93～100 ℃ of hot water, promptly finished the pre-agglomeration process of glue;
The control residence time was 40～50 minutes under glue after d, the pre-cohesion continued to stir in the cohesion still, promptly finished the elutriation method agglomeration process.
Embodiment 9
Agglomerating solution-polymerized rubber device of the present invention is to be made of steam heater 1, glue mixing tank 2, pre-lime set nozzle 3 and cohesion still 4,5.The outlet line of steam heater 1 is connected with glue mixing tank 2 pipelines, and the outlet of glue mixing tank 2 connects pre-lime set nozzle 3, and the outlet of pre-lime set nozzle 3 places cohesion still 4, and the outlet line of cohesion still 4 is connected with cohesion still 5 through pump 6.Wherein, dispersion agent inlet c, alkali liquor inlet d and glue inlet e are arranged having on the steam heater 1 on recirculated water inlet a and steam-in b, its outlet line; Recirculated water inlet f and steam-in g are arranged on cohesion still 4; Steam-in i, gas phase precipitate outlet j and micelle water out k are arranged on cohesion still 5.
Claims (5)
1. method for agglomerating solution-polymerized rubber, its feature comprises following operation steps:
A, heat water to 115 ℃～130 ℃ and make superheated water, and add polycarboxylic acid sodium dispersion agent and sodium hydroxide lye, the dispersion agent add-on is 1 * 10 of a dry glue quality
-4～5 * 10
-4, alkali lye add-on to the pH value of control cohesion hot water is between 9～10;
B, with the superheated water solution thorough mixing that glue and a step make, obtain the non-homogeneous mixture of 113 ℃～125 ℃ of glue-hot water;
C, glue-hot water non-homogeneous mixture sprayed be injected with in the cohesion still of 93～100 ℃ of hot water, promptly finished the pre-agglomeration process of glue;
The control residence time was 40～50 minutes under glue after d, the pre-cohesion continued to stir in the cohesion still, promptly finished the elutriation method agglomeration process.
2. method for agglomerating solution-polymerized rubber as claimed in claim 1 is characterized in that the mixed volume ratio of glue and superheated water is 1: 2～3 in the b step.
3. method for agglomerating solution-polymerized rubber as claimed in claim 1 is characterized in that the spraying pressure in the c step is 0.4MPa～0.8MPa.
4. described method for agglomerating solution-polymerized rubber as claimed in claim 1 is characterized in that condensing in the d step elutriation method agglomeration process still (4) temperature and is controlled at 93 ℃～99 ℃, pressure-controlling at 0.06MPa～0.10MPa; Cohesion still (5) temperature is controlled at 96 ℃～102 ℃, pressure-controlling at 0.02MPa～0.04 MPa.
5. the agglomerating solution-polymerized rubber device is to be made of steam heater (1), glue mixing tank (2), pre-lime set nozzle (3) and cohesion still (4), (5), the outlet line that it is characterized in that steam heater (1) is connected with glue mixing tank (2) pipeline, the outlet of glue mixing tank (2) connects pre-lime set nozzle (3), the outlet of pre-lime set nozzle (3) places cohesion still (4), and the outlet line of cohesion still (4) is connected with cohesion still (5) through pump (6); Wherein, dispersion agent inlet c, alkali liquor inlet d and glue inlet e are arranged having on the steam heater (1) on recirculated water inlet a and steam-in b, its outlet line; Recirculated water inlet f and steam-in g are arranged on cohesion still (4); Steam-in i, gas phase precipitate outlet j and micelle water out k are arranged on cohesion still (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101593540A CN101235105B (en) | 2007-12-30 | 2007-12-30 | Method for agglomerating solution-polymerized rubber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101593540A CN101235105B (en) | 2007-12-30 | 2007-12-30 | Method for agglomerating solution-polymerized rubber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101235105A true CN101235105A (en) | 2008-08-06 |
| CN101235105B CN101235105B (en) | 2010-06-23 |
Family
ID=39919040
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007101593540A Expired - Fee Related CN101235105B (en) | 2007-12-30 | 2007-12-30 | Method for agglomerating solution-polymerized rubber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101235105B (en) |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565471B (en) * | 2009-05-22 | 2010-11-10 | 孙建军 | Energy-saving method of synthetic rubber technique and equipment thereof |
| CN102181002A (en) * | 2011-03-04 | 2011-09-14 | 中国石油天然气股份有限公司吉林石化分公司 | Wet coagulation method for rare-earth isoprene rubber |
| CN102382214A (en) * | 2011-08-31 | 2012-03-21 | 中国石油化工股份有限公司 | Coacervation technology for polymer product production |
| CN102040676B (en) * | 2009-10-23 | 2013-01-09 | 中国石油化工股份有限公司 | Method for depriving solvent for cis-polybutadiene |
| CN104072643A (en) * | 2013-03-28 | 2014-10-01 | 中国石油化工股份有限公司 | Method for removing solvent from solution-polymerized polymer |
| CN104961846A (en) * | 2015-07-03 | 2015-10-07 | 新疆蓝德精细石油化工股份有限公司 | Apparatus for improving separation effect of rubber oil in coagulation step and application method thereof |
| CN105777945A (en) * | 2014-12-17 | 2016-07-20 | 中国石油化工股份有限公司 | Polyolefin glue solution agglomeration method |
| CN106032394A (en) * | 2015-03-17 | 2016-10-19 | 中国石油化工股份有限公司 | Polyisoprene rubber production method, and polyisoprene rubber and applications thereof |
| CN106540472A (en) * | 2015-09-22 | 2017-03-29 | 中国石油化工股份有限公司 | The condensing method of rubber polymer condensing field and coacervation device and rubber polymer solution |
| CN112111027A (en) * | 2019-06-20 | 2020-12-22 | 中国石油化工股份有限公司 | Double-kettle coagulation method for isoprene rubber solution |
| CN112125988A (en) * | 2019-06-24 | 2020-12-25 | 中国石油化工股份有限公司 | Coagulation method for styrene thermoplastic elastomer solution |
| CN112142876A (en) * | 2019-06-27 | 2020-12-29 | 中国石油化工股份有限公司 | Method for coagulating butadiene rubber solution |
| CN112142877A (en) * | 2019-06-27 | 2020-12-29 | 中国石油化工股份有限公司 | Coagulation method for butadiene rubber solution |
| CN114316090A (en) * | 2020-09-29 | 2022-04-12 | 北京诺维新材科技有限公司 | Low-solvent-residue polymer and preparation method thereof |
| CN114426589A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | Production method of butadiene rubber |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1388400A1 (en) * | 1985-10-29 | 1988-04-15 | Предприятие П/Я В-8783 | Method of separating butadiene rubber |
| SU1745729A1 (en) * | 1989-09-18 | 1992-07-07 | Нижнекамское производственное объединение "Нижнекамскнефтехим" | Method of process control in separation of synthetic rubber from solutions |
| US5316659A (en) * | 1993-04-02 | 1994-05-31 | Exxon Research & Engineering Co. | Upgrading of bitumen asphaltenes by hot water treatment |
| CN100453586C (en) * | 2007-04-13 | 2009-01-21 | 青岛伊科思新材料股份有限公司 | Steam stripping coacervation and separation device for polymer solution and separation method thereof |
-
2007
- 2007-12-30 CN CN2007101593540A patent/CN101235105B/en not_active Expired - Fee Related
Cited By (28)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565471B (en) * | 2009-05-22 | 2010-11-10 | 孙建军 | Energy-saving method of synthetic rubber technique and equipment thereof |
| CN102040676B (en) * | 2009-10-23 | 2013-01-09 | 中国石油化工股份有限公司 | Method for depriving solvent for cis-polybutadiene |
| CN102181002A (en) * | 2011-03-04 | 2011-09-14 | 中国石油天然气股份有限公司吉林石化分公司 | Wet coagulation method for rare-earth isoprene rubber |
| CN102181002B (en) * | 2011-03-04 | 2012-11-14 | 中国石油天然气股份有限公司吉林石化分公司 | Wet coagulation method for rare-earth isoprene rubber |
| CN102382214A (en) * | 2011-08-31 | 2012-03-21 | 中国石油化工股份有限公司 | Coacervation technology for polymer product production |
| CN102382214B (en) * | 2011-08-31 | 2013-04-03 | 中国石油化工股份有限公司 | Coacervation technology for polymer product production |
| CN104072643A (en) * | 2013-03-28 | 2014-10-01 | 中国石油化工股份有限公司 | Method for removing solvent from solution-polymerized polymer |
| CN104072643B (en) * | 2013-03-28 | 2016-09-14 | 中国石油化工股份有限公司 | The method containing intermingle with polymer desolvation |
| CN105777945B (en) * | 2014-12-17 | 2017-06-06 | 中国石油化工股份有限公司 | A kind of method of polyolefin glue cohesion |
| CN105777945A (en) * | 2014-12-17 | 2016-07-20 | 中国石油化工股份有限公司 | Polyolefin glue solution agglomeration method |
| CN106032394A (en) * | 2015-03-17 | 2016-10-19 | 中国石油化工股份有限公司 | Polyisoprene rubber production method, and polyisoprene rubber and applications thereof |
| CN106032394B (en) * | 2015-03-17 | 2017-08-22 | 中国石油化工股份有限公司 | The production method and isoprene rubber of a kind of isoprene rubber and its application |
| CN104961846A (en) * | 2015-07-03 | 2015-10-07 | 新疆蓝德精细石油化工股份有限公司 | Apparatus for improving separation effect of rubber oil in coagulation step and application method thereof |
| CN104961846B (en) * | 2015-07-03 | 2017-03-08 | 新疆蓝德精细石油化工股份有限公司 | Improve device and its using method of cohesion process rubber oil separating effect |
| CN106540472B (en) * | 2015-09-22 | 2018-12-28 | 中国石油化工股份有限公司 | The condensing method of rubber polymer condensing field and coacervation device and rubber polymer solution |
| CN106540472A (en) * | 2015-09-22 | 2017-03-29 | 中国石油化工股份有限公司 | The condensing method of rubber polymer condensing field and coacervation device and rubber polymer solution |
| CN112111027B (en) * | 2019-06-20 | 2022-08-19 | 中国石油化工股份有限公司 | Double-kettle coagulation method for isoprene rubber solution |
| CN112111027A (en) * | 2019-06-20 | 2020-12-22 | 中国石油化工股份有限公司 | Double-kettle coagulation method for isoprene rubber solution |
| CN112125988A (en) * | 2019-06-24 | 2020-12-25 | 中国石油化工股份有限公司 | Coagulation method for styrene thermoplastic elastomer solution |
| CN112125988B (en) * | 2019-06-24 | 2023-04-11 | 中国石油化工股份有限公司 | Coagulation method for styrene thermoplastic elastomer solution |
| CN112142877A (en) * | 2019-06-27 | 2020-12-29 | 中国石油化工股份有限公司 | Coagulation method for butadiene rubber solution |
| CN112142876B (en) * | 2019-06-27 | 2022-08-19 | 中国石油化工股份有限公司 | Method for coagulating butadiene rubber solution |
| CN112142877B (en) * | 2019-06-27 | 2022-09-20 | 中国石油化工股份有限公司 | Coagulation method for butadiene rubber solution |
| CN112142876A (en) * | 2019-06-27 | 2020-12-29 | 中国石油化工股份有限公司 | Method for coagulating butadiene rubber solution |
| CN114316090A (en) * | 2020-09-29 | 2022-04-12 | 北京诺维新材科技有限公司 | Low-solvent-residue polymer and preparation method thereof |
| CN114316090B (en) * | 2020-09-29 | 2023-06-30 | 北京诺维新材科技有限公司 | Polymer with low solvent residue and preparation method thereof |
| CN114426589A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | Production method of butadiene rubber |
| CN114426589B (en) * | 2020-10-29 | 2023-10-20 | 中国石油化工股份有限公司 | Production method of butadiene rubber |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101235105B (en) | 2010-06-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101235105B (en) | Method for agglomerating solution-polymerized rubber | |
| CN102451572B (en) | Method for separating acetic acid from water by rectification of acetic acid dehydrating tower | |
| CN202808649U (en) | Systemic device for preparing polyoxymethylene dimethyl ether | |
| CN102451573B (en) | Acetic acid dehydrating tower rectifying method | |
| CN101462953A (en) | Method for preparing pentaerythritol triacrylate | |
| CN105669362A (en) | Trichloromethane solvent recovery heat pump rectification process | |
| CN104817481A (en) | Technological method for recovering DMSO from DMSO aqueous solution | |
| CN107235939A (en) | With the method for improving furaldehyde yield in a kind of aldehyde vapour gas phase | |
| CN114988453B (en) | Nanometer calcium carbonate production device and production method | |
| CN104072643A (en) | Method for removing solvent from solution-polymerized polymer | |
| CN102584751B (en) | Process and reaction system for preparing furfuraldehyde by reaction rectification method | |
| CN111233690A (en) | DMAc thermal coupling refining and recycling system and method | |
| CN205740829U (en) | Extend methylamine catalyst and use the catalyst application apparatus in cycle | |
| CN104781425B (en) | Instantaneous cooling for biomass material hydrolysis to be quenched | |
| CN100384717C (en) | Insoluble sulfur preparation | |
| CN105910483B (en) | Natural Circulation boiling heat transfer reclaims the method that pasty material waste heat and heating are utilized | |
| CN105439823B (en) | A kind of method for synthesizing the alcohol of 3 methyl, 3 butylene 1 | |
| CN104140357B (en) | Take acetic acid as the method for raw material production ethanol | |
| CN105713113B (en) | Method for recovering heat of gas-phase material in condensation kettle | |
| CN113402010A (en) | Safe, energy-saving and efficient 'three-high' wastewater treatment process | |
| CN103772153B (en) | The synthetic method of the chloro-3-cresols of 4-and system thereof | |
| CN103936601B (en) | ammonia recovery method in ethanolamine production | |
| CN101580285A (en) | Thermal cracking device for papermaking black liquor of non-wood material | |
| CN206843352U (en) | A kind of 1,4 butynediols purification systems | |
| CN101462952A (en) | Method for preparing neopentylglycol diacrylate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100623 Termination date: 20161230 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |