CN1033643A

CN1033643A - Automatically circulation formula continuous processing is produced clorafin and chlorocarbon technology and main device

Info

Publication number: CN1033643A
Application number: CN 87108178
Authority: CN
Inventors: 楼存宝
Original assignee: Individual
Current assignee: Individual
Priority date: 1987-12-18
Filing date: 1987-12-18
Publication date: 1989-07-05

Abstract

Automatically circulation formula continuous processing is produced the production technique of clorafin and chlorocarbon, is with chlorine and straight chain hydrocarbon mixture oils, by reactor and one group of barrel type reactor that is installed in series, reacts continuously.Hydrogen chloride gas water that produces or weak hydrochloric acid absorb by-product hydrochloric acid, and the utilization ratio that makes chlorine is up to 98%.Utilize this technology will increase substantially throughput, reduce labor intensity.The employed stock oil of this technology, except that normally used whiteruss and solid paraffin, can also be with other straight chain hydrocarbon mixture oils.Opened up the production approach.Product can be used for softening agent, the additive of lubricating oil, machine oil etc., fire retardant etc.

Description

Automatically circulation formula continuous processing is produced clorafin and chlorocarbon technology and main device

Automatically the technology of circulation formula continuous processing production clorafin and chlorocarbon belongs to vitochemical manufacture method.

The traditional technology of existing production clorafin is interrupter method production, with melt paraffin or whiteruss less than 0.1MPa pressure, be lower than 95 ℃ of logical chlorine below the temperature, treat that proportion is increased to certain value, when promptly reaching desired chlorinity, logical pressurized air purges, and removes hydrogen chloride gas, promptly gets product.There is following defective in this technology, and the one, the production cycle is grown (generally each pot is produced from feeding intake and made finished product needs 30～40 hours), and throughput is low, does not satisfy the social demand that increases day by day; The 2nd, chlorine utilization is low, has only 75～80%, and rest part enters atmosphere, promptly wastes raw material and contaminate environment; The 3rd, interrupter method is produced the requirement height of clorafin technology to stock oil, must select for use normal paraffin (paraffin) cost height, the source of purity more than 95% few, has hindered the development of producing.

In order to overcome the shortcoming that existing production technique exists, seek continuous production technology, seek to adapt to the processing method of many kinds oils as raw material, become our research topic.Through experimental study repeatedly, trial-produce the novel process of " formula that circulates automatically continuous processing is produced clorafin or chlorocarbon " finally successfully.

Main flow process of the present invention is divided into four technologies, and the one, stock oil is refining, and the 2nd, for the chlorine operation, the 3rd, chloride process, the 4th, absorb operation.Wherein stock oil is refining.For chlorine and absorption operation, be known prior art, do not give unnecessary details for this reason.

Fig. 1 is the schema of chloride process.

Feedstock oil enters reaction pot (13) from head tank (1), and chlorine passes into reaction pot bottom by chlorine separator (14), and namely plays chlorination reaction after feedstock oil contact, and the reactant liquor liquid level constantly rises, liquid level arrival When giving vent to anger the mouth of pipe, reactant liquor is brought gas-liquid separator (2) into by the hydrogen chloride gas that chlorination reaction generates, and tail gas (containing chlorine and hydrogen chloride gas) enters reactor (9), and reactant liquor then enters reactor (7) bottom. In the reactant liquor of this device, pass into again fresh chlorine, gas-liquid is imported this device continuously, automatically enter in the gas-liquid separator (3) from this device top continuously, tail gas then from device top with (2) and the tail gas that comes enters reactor (9) simultaneously, reactant liquor then enters the bottom of reactor (8), leads to for the third time chlorine, so that further chlorination.

Is a bank of reactor from (9) to (10), fills the porcelain circle, with the contact area of increase gas-liquid two-phase, and reaction solution and chloride tail gas coflow, adjacent two reactors circulate automatically according to its pressure reduction.

From the reaction solution that reactor (10) comes out, because of containing the hydrogenchloride of volume.Enter reactor (11), (12) again, purge with the air for continuous of coming from air distributor (15), the reaction solution (being the finished product chlorocarbon) that comes out from separator (6) flows into the finished product storage (16), and the tail gas of going out from separator (5), (6), remove to absorb process water or light hydrogenchloride liquid and absorb, make by-product hydrochloric acid.

In reaction process, it is that pressure is enough to overcome intrasystem resistance and keeps reaction that the reactor internal pressure is controlled at less than 0.1MPa(), temperature is controlled at 90 ℃～95 ℃.The throughput ratio of stock oil and chlorine (volumetric flow rate) remains on

When producing the chlorinated paraffin-42 product is 1: 350～400

When producing the chlorinated paraffin-52 product is 1: 520～600

Because material residence time in reactor is short, reaction not exclusively, the reaction solution that reactor is come out for this reason, through gas-liquid separator, reaction solution and gas mixture enter one group of reactor that is installed in series again.The structure of reactor as shown in Figure 2, it is the barrel type reactor that has chuck (2), flange (1) is equipped with at two ends up and down, porous plate (6) is equipped with in the lower end of inner core (3), huddles porcelain circle (4) on porous plate, to increase the gas-liquid two-phase contact area.Logical water coolant in the chuck, to keep temperature of reaction, water coolant is by taking over (5) turnover.

In reactor, the gas-liquid two-phase coflow, reactors in series is installed, according to the quantity of chlorination degree decision tandem reactor.Glass or transparent material are adopted in the import and export of reactor.Reactor is peripherally equipped with fluorescent lamp, further quickens chlorination reaction under the katalysis of light.

The processing condition of reactor:

The pressure of first reactor of import generally is controlled between 0.05～0.09MPa less than 0.1MPa, and two adjacent reactors circulate automatically according to its pressure reduction.

Temperature of reaction is no more than 95 ℃ in all reactors, generally is controlled at 80～90 ℃

The chlorinated hydrocarbons product that utilizes this technology to make, advantage such as it is low to have freezing point, and flame retardant resistance is strong, and mutual solubility is good, and weight loss on heating is little can replace time dioctyl phthalate (DOP), and dibutylester is as the softening agent of plastics.

Compare with existing interrupter method production technique, the present invention has throughput big (whole chlorination reaction can be finished at 15 minutes), chlorine utilization height (can reach about 98%), and environmental pollution is little.This technology except available whiteruss and solid paraffin, can also have been opened up raw materials market to the claimed range broad of stock oil with other illuminating kerosene, light coal oil, ink oil, content of wax wet goods straight chain hydrocarbon mixture in addition.

Below in conjunction with embodiment, further specify the present invention.

Embodiment 1

Through the special ink oil of refinement treatment, with 0.4 liter of/minute reactor that feeds 300 liters of flow, the flow control of chlorine is at 220 liters/minute, pot inner pressure 0.06MPa, 95 ℃ of temperature of reaction, by the reaction solution that reactor comes out, 14 reactors that are installed in series are gone in circulation automatically.After 15 minutes, get final product to such an extent that be yellowish chlorocarbon product: chlorinated paraffin-52.

Embodiment 2

Witco 70 feeds the reactor of 300 liters with 0.51 liter/minute of flow, 180 liters/minute of chlorine flowrates, and pot inner pressure 0.09MPa, temperature of reaction is at 90 ℃.By the reaction solution that reactor comes out, flow into 12 reactors that are installed in series automatically, after 15 minutes, can get product: chlorinated paraffin-42.

Claims

1, a kind of technology of producing clorafin and chlorocarbon, its production method be with paraffin less than 0.1MPa pressure, be lower than logical chlorine under 95 ℃ the temperature, when treating that proportion is increased to certain value, when promptly reaching desired chlorinity, logical pressurized air purges, and removes hydrogen chloride gas.It is characterized in that: through purified stock oil and chlorine, generate the spumescence reaction solution by reactor, through gas-liquid separator and one group of barrel type reactor, the whole process of chlorination reaction is that automatic circulation is carried out continuously.

2, the technology of producing clorafin and chlorocarbon by the described automatic circulation formula continuous processing of claim 1, the processing condition of its reactor are control stock oil: the volume flow ratio of chlorine

When producing the chlorinated paraffin-42 product is 1: 350～400

When producing the chlorinated paraffin-52 product is 1: 520～600

3, by the described technology of claim 1, the processing condition of its first barrel type reactor are:

Working pressure generally is controlled at 0.05～0.09MPa less than 0.1MPa

Service temperature is at 80 ℃～90 ℃

Reaction solution and chlorine coflow in device, two adjacent reactors circulate automatically according to its pressure reduction.

4, by the described production technique of claim 1, used stock oil can also be with other straight chain hydrocarbon mixture oils except that general whiteruss and solid paraffin.

5, circulate automatically that the formula continuous processing is produced clorafin and the required reactor of chlorocarbon is characterized by: have the barrel type reactor of chuck, logical water coolant in the chuck, porous plate is equipped with in the container lower end, huddles the porcelain circle on it, and reactors in series is installed.