SU1432067A1 - Method of producing polymeric flocculant - Google Patents

Abstract

The invention relates to a process for the production of polymer flocculant used to clean the oilfield waters of oil fields. An increase in the efficiency of flocculation is achieved by copolymerization of piperylene, maleic anhydride and styrene at a molar ratio of 1.2: 1: 0.1 to 2.6: 1.5: 1.5, respectively. The copolymerization process is carried out at 49.5-50.5 C in acetone. Dicyclohexyl peroxydicar bonate is used as a happy PCL initiator during its polymerization. 1 hp f-ly, 2 tab. 4 CO 1 hE O 05-x |

Description

This invention relates to a process for the preparation of polymer flocculant for the purification of oil field waters of oil fields. Example 1 Copolymerization of 2.6 moles of piperylene (PP), 1.0 moles of maleic anhydride (MA) and moles of styrene (CT) are carried out in large ampoules. YU

The reaction mixture in the ampoule is frozen in liquid nitrogen and evacuated to a residual pressure of mm Hg. to remove

dissolved in the monomers of oxygen 15 vskhtukha. The operation of freezing, -,: ia-kug-girovayie - razmorachivaglie repeated two or three times. Then the vial otpaivat and immediately placed in a thermostat. The temperature is maintained at 20 50tO ,. The copolymers are isolated by precipitation from an acetone solution in sulfuric ether. The ratio of solution and precipitant is 1:10 - 1:15. The copolymerization products are cleaned by extracting 25 with toluene in a Soxhlet apparatus to remove unreacted MA and Diels-Alder adduct (product of the interaction of MA with III). After purification, the copolymers are dried in a vacuum in the mind (1 mm Hg) at 45–50 ° C. The IR spectra of the copolymers contain absorption bands characteristic of three comonomers: PP - (735-740, cm cis-C-bond; 960 trans-C-bond); benzene ring (1500, 1610), NA - (1760, 1870 cm-).

The synthesis conditions and properties of the copolymers are given in Table. 1. Q

To obtain a water soluble copolymer analogue, the polymer obtained is subjected to ammonolysis. Ammonolysis is carried out

in a three-necked flask5 equipped with a stirrer, a reflux condenser, and a tube j for bubbling ammonia gas. Gaseous ammonia is obtained by boiling and not drying.

The polymer is suspended in benzene -. (30% copolymer and 70% benzene), ammonia is bubbled through the slurry. The reaction temperature of the modification is maintained at 50iO, 5 C. The reaction time is 2-5 hours. The modified copolymers are filtered off with acetone and reduced to constant weight in vacuum at 50 s.

After ammonolysis, in the IR spectra of the products, the absorption bands characteristic of PP and CT were retained; there were no bands. absorption, characteristic. for MA and absorption bands appeared in the region of 1550 cm (carboxylate anion COO),: 1675 (the second

amide band - C) 1705 (carN l

Boxing group SOOP). The presence of ammonium nitrogen is determined by potentiometric titration of aqueous solutions of polymers, 0.1N HCl solution in the presence of a mixed indicator.

Examples 2-5. The method is carried out analogously to example 1.

The duration of the process, the composition of the monomer mixture and some properties of the polymers are given in table. one.

The flocculating properties of PMAS are determined according to a known method as follows: the water to be purified is poured into 1 liter glasses, the coagulant solution (alkaline agent) is introduced gradually, by adding to the waste water in small portions. K.azh, again after pH check. Coagulant is added until the pH of the solution is 7.5 or 8.2. After reaching this pH value, for a short time, observe the changes taking place in the beaker. If there are no changes, then with stirring at a speed of 60-70 s b / min, flocculents in an amount of from 0.25 to 100 mg / l are added with a pipette. Stir at this speed for 2 minutes, then reduce the rotation speed of the stirrer to 30 v / min. mix for another 5 minutes. The broom switch is turned off, the blades of the agitator are lifted from the glasses and the flocculation is observed, and after some time the sedimentation of the precipitate takes place. Obtain the turbidity reading (after 15, 30, 45, 60 min). From each glass from a certain height of the liquid column is taken with a piston pipette 25 ml of the test water. This liquid is poured into numbered cups.

The test and distilled water is poured into the cuvettes and the turbidimeter is recorded.

In addition, monitor the concentration of oil and mechanical impurities.

Purification efficiency is determined on oil field waters, which contain, mg / l: petroleum products up to 1300; mechanical impurities up to 500-700; iron sulfide up to 330,

To use these flows in the system of maintaining the plast pressure, it is necessary to reduce the content, mg / l: petroleum products to 10-20; mechanical impurities and iron sulfide (in total) up to 15-20.

Such a content of said suspended particles (oil products, mechanical impurities and iron sulfide) corresponds to a degree of clarification of 98-99%.

Claims (1)

1. A method of producing polymer flocculant by copolymerizing a monomeric mixture containing maleic anhydride and styrene in acetone in the presence of a radical initiator pr and 49.5-50, followed by treatment with ammonia, characterized in that, in order to ensure the effectiveness of flocculant during purification waste oil field waters; in the composition of the monomer mixture, piperylene is additionally used at the following molar ratio of components: piperylene: maleic anhydride: styrene from 1.2: 1: 0.1 to 2.6: 1.5: 1.5, respectively. about tl and h a- as pa2. The method according to claim 1, y and i with the fact that dicyclohexyl peroxydicarbonate is used in the dical initiator, 2.6 1.0 1.5 3.5 80.1 5.2 A9.6 A5.2 2.6 1.2 4 (control.) 1.0 1,51,04,076,416,0052,531,50,48 1,00,1 S, 5 59,536,457,85; 80,61 g, 0- -4.545, 5458.46-0.38 Ras1voii- Nerastvo- Dissolve-Nerastvo-Norast-Solstvo-Nerastimymymymymymyvorimy r: 1my , Table 1 0.54 Continuation of the table 4 (CONTROL) 5 (x-terminal ; by i- (Vest: J way) i, 1. 3  The concentration of dicyclohexyl peroxydicarbonate is 0.5% by weight per 100% by weight. monomers. The comonomer concentration in acetone is 15 mas. Temperature copolymerization of 49.5-50.5 C. XX. Decomposition temperature of products C. Continuation of table 1 table 2 m 1432067 12 Continued table. 2