CN1970519A - Nonyl phenol refining process - Google Patents

Nonyl phenol refining process Download PDF

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CN1970519A
CN1970519A CN 200510123489 CN200510123489A CN1970519A CN 1970519 A CN1970519 A CN 1970519A CN 200510123489 CN200510123489 CN 200510123489 CN 200510123489 A CN200510123489 A CN 200510123489A CN 1970519 A CN1970519 A CN 1970519A
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nonylphenol
phenol
distillation
temperature
process
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CN 200510123489
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CN100486947C (en )
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张耀亨
邵鹏程
张霖
姚亚平
盛刚
王桂敏
高维娜
延小平
梁乐
赵琳
赵力
董建军
李长伟
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中国石油天然气集团公司
中国石油兰州石油化工公司
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Abstract

The invention discloses a refining technique to synthesize industrial nonyl phenol, which comprises the following steps: a) evaporating to remove most of phenol in the industrial nonyl phenol; obtaining evaporator bottom material; b) distilling to remove phenol; obtaining rough nonyl phenol; setting the temperature of feed material into distill tower at 70-120 deg.c and tower top temperature at 40-85 deg.c and tower autoclave temperature at 170-215 deg.c; setting the total fill pressure at 0.4-1.0Kpa; controlling the reflux rate R between 0.5 and 2; obtaining the theoretical tower boards at 6-30 blocks; c) rectifying the rough nonyl phenol to obtain refined nonyl phenol and rough dinonyl phenol; setting the feed temperature of rectifying tower at 90-130 deg.c and tower top temperature at 80-170 deg.c and tower autoclave temperature at 180-260 deg.c; setting the total fill pressure at 0.4-1.0Kpa; controlling the reflux rate R between 0.4 and 2.5; obtaining the theoretical tower boards at 4-28 blocks.

Description

一种壬基酚精制工艺 One kind of refining process nonylphenol

技术领域 FIELD

本发明涉及工业壬基酚的精制工艺,特别涉及一种由壬烯和苯酚在催化剂的作用下合成的工业壬基酚的精制工艺。 The present invention relates to a process of refining industry nonylphenol, and in particular relates to a process for the purification of phenol and nonene synthesis catalyst under industrial nonylphenol.

背景技术 Background technique

工业壬基酚是由壬烯和苯酚在催化剂的作用下化合而成的,但是由于各种原因,工业生产的壬基酚产品很容易在贮存过程中或是在下游产品的生产过程中氧化变色,有时这种变色过程十分迅速,直接影响了壬基酚的销售和使用。 Industrial nonylphenol compounds are formed in the catalyst by phenol and nonene, but for various reasons, the production of industrial products easily nonylphenol or oxidative discoloration in the course of downstream products during storage sometimes this discoloration process is very rapid, direct impact on the marketing and use of nonylphenol. 国产壬基酚产品在室温下放置12天,色泽可由47Hazen变为500Hazen以上。 Products made nonylphenol for 12 days at room temperature, the color may be changed 500Hazen 47Hazen above. 上海石化研究院的实验室研究发现,当壬基酚纯度较高,苯酚含量低、产品纯度高时,色泽度低,色泽稳定性好。 Shanghai Petrochemical Research Institute laboratory study found that when nonylphenol high purity, low phenol content, high product purity, the low degree of color, good color stability. 壬基酚色泽稳定性下降是由于产品中的杂质引起的,尤其是残余苯酚,其次低碳数烷基酚和二壬基酚,会对壬基酚色泽及其稳定性造成不利影响。 Nonylphenol color stability is decreased due to the product due to impurities, especially residual phenol, followed by the lower number of adverse effects and alkylphenol dinonylphenol, will nonylphenol and color stability. 黑龙江石油化工厂设计室发现产品纯度高、色度低,不易变色,存放时间长。 Heilongjiang petrochemical plant designs chamber found that high purity, low color, difficult to change, stored for a long time. 因此降低壬基酚产品中的杂质,特别是残余苯酚对于提高色泽稳定性有重要的意义。 Nonylphenol thus reducing impurities in the product, especially for improving the color stability of the residual phenol has important significance.

据了解,在苯酚回收和壬基酚精制的过程中,普遍存在着产品回收率低的问题。 It is understood that nonylphenol phenol recovery and refining process, the prevalence of low product recovery problems. 产品壬基酚中苯酚含量高,二壬基酚没有得到很好的回收利用。 High phenol content product nonylphenol, dinonylphenol not well recycled.

在现有专利文献中没有发现采用“蒸发—蒸馏—精馏—间歇蒸馏”四步法工艺回收苯酚和精制壬基酚的技术文献报导,比如专利CN1082530A,US5300703。 Is not found in the prior patent literature a "evaporation - Distillation - Distillation - batch distillation" four step process and purified nonyl phenol recovery techniques reported in the literature, such as patents CN1082530A, US5300703. 国内外现有的关于回收苯酚和精制壬基酚的技术有波兰布兰科尼尔有机合成研究院的专利技术、德国Hüels公司回收工艺和由兰州石化分公司开发的回收和精制工艺。 Existing techniques for the recovery and purification of phenol nonylphenol domestic and foreign patents Polish Academy Blanco denier of organic synthesis, the recovery process and the German company Hüels Lanzhou Petrochemical Branch developed by the recovery and purification process. (1)波兰技术:由图1可知,回收部分首先采用薄膜蒸发器蒸发,脱出大部分的苯酚,被脱除苯酚返回壬基酚合成系统循环,塔釜流出物进入蒸馏塔,然后采用间歇蒸馏的方式,获得壬基酚。 (1) Technology Poland: Figure 1 shows, the recovery section is first evaporated using a thin film evaporator, most prolapse phenol, phenol is removed nonylphenol synthesis system return cycle, the bottoms effluent enters the distillation column, and a batch distillation the way, nonylphenol. 该工艺的缺点是:a产物壬基酚内残余酚含量高;b循环苯酚内含壬基酚;c釜残液中壬基酚含量很高。 A disadvantage of this process is: a product of the high content of residual phenol nonylphenol; B containing cyclic phenol nonylphenol; c bottoms nonylphenol high content. (2)Hüels公司技术:由图2可知,回收工艺中首先将低碳烃类蒸馏出来回收,塔釜流出物通过蒸发塔蒸发,脱出大部分苯酚,被脱出的苯酚返回到壬基酚合成系统循环,塔釜流出物进入精馏塔,产物壬基酚从塔顶蒸出,二壬基酚作为侧线分离出来,返回到壬基酚合成装置中,因此二壬基酚纯度差,不能作为专门的产物,只能用于烷基转移。 (2) Hüels Technical: Figure 2 shows, the recovery process is first distilled off lower hydrocarbon recovery bottoms by evaporation column effluent evaporation, most of phenol prolapse, prolapse phenol is returned to the synthesis system nonylphenol cycle, into the fractionator bottoms effluent, the product distilled from the column top nonylphenol, dinonylphenol isolated as a side, to return to the synthesis apparatus nonylphenol, dinonylphenol poor purity and therefore, can not serve as special product, only for transalkylation. 二壬基酚没有得到很好的回收利用。 Dinonylphenol not well recycled. (3)兰州石化分公司技术:由图3可知,回收部分采用连续蒸馏脱酚、连续精馏获得产品壬基酚的方法。 (3) Technology Lanzhou Petrochemical Branch: seen from Figure 3, part of a continuous distillation method using phenol removal, continuous distillation for product recovery nonylphenol. 工艺的缺点是:a脱酚塔分离要求过高,难以兼顾塔顶和塔底物料的分离要求;b壬基酚精馏塔分离要求过高,为了保障壬基酚产品质量,造成塔底物料含有大量壬基酚。 Shortcoming process are: too high a phenol removal tower separation requirements, taking into account the difficult separation requirements overhead and bottoms material; b nonylphenol distillation column separation requirements too high, in order to guarantee product quality nonylphenol, resulting bottoms It contains a lot of nonylphenol.

发明内容 SUMMARY

对于由壬烯和苯酚在催化剂的作用下化合而成的工业壬基酚精制,本发明提供一种新的壬基酚精制和新的二壬基酚回收组合工艺技术。 For the compound in the catalyst formed by nonene and phenol nonylphenol refining industry, the present invention provides a novel purified and nonylphenol dinonylphenol new recovery technology combinations. 工艺包括蒸发脱除大部分苯酚、蒸馏脱残酚、壬基酚精馏和间歇蒸馏获得二壬基酚四个工艺步骤。 Removal of most of the phenol processes include evaporation, distillation residue removal, nonylphenol batch distillation and distillation to obtain a dinonyl four step process. 依靠本发明的工艺,改善了产品壬基酚的色泽稳定性、增加了产品收率。 By either process of the present invention improves the color stability of the product of nonylphenol, increased product yield.

本发明的目的是通过一种新的壬基酚精制工艺(概括为“蒸发—蒸馏—精馏—间歇蒸馏”四步法工艺)的实施,能快速有效的将壬基酚中的酚含量降至很低,同时进一步提高壬基酚的收率,回收利用二壬基酚。 Object of the present invention is achieved by a new refining process nonylphenol (summarized as "evaporative - Distillation - Distillation - batch distillation" four-step process) of the embodiment can be quickly and effectively reduce the content of the phenol nonylphenol to low, while further improving the yield of nonylphenol, dinonylphenol recycling. 具体发明技术内容为:一种壬基酚精制工艺,精制壬烯和苯酚在催化剂的作用下化合而成的工业壬基酚,其特征在于:包括以下过程,a)蒸发:去除工业壬基酚中的大部分苯酚,得到蒸发器底部出料;b)蒸馏:去除蒸发器底部出料中的苯酚,得到粗壬基酚,蒸馏塔进料温度为70℃~120℃,塔顶温度为40℃~85℃,塔釜温度为170~215℃,总填料压力降为0.4Kpa~1.0Kpa,回流比R控制在0.5~2之间,理论塔板数为6~30块;c)精馏:精馏粗壬基酚,得到精制壬基酚和粗二壬基酚,精馏塔进料温度为90℃~130℃,塔顶温度为80℃~170℃,塔釜温度为180~260℃,总填料压力降为0.4Kpa~1.0Kpa,回流比R控制在0.4~2.5之间,理论塔板数为4~28块。 Specific technical contents of the invention: one kind of nonylphenol refining process, refined nonene and phenol compound in the presence of a catalyst obtained by industrial nonylphenol, characterized by: comprising the following process, A) Evaporation: Industrial nonylphenol removed most phenol, bottom discharge was evaporated; b) distillation: removing the bottom of the evaporator feed phenol, nonyl phenol to give a crude distillation column feed temperature of 70 ℃ ~ 120 ℃, column top temperature of 40 ℃ ~ 85 ℃, tower bottom temperature is 170 ~ 215 ℃, the total pressure drop packing 0.4Kpa ~ 1.0Kpa, controlling the reflux ratio R between 0.5 and 2, the theoretical plate number is from 6 to 30; c) distillation : crude distillation nonylphenol, nonylphenol and purified to give the crude dinonylphenol, fractionator feed temperature of 90 ℃ ~ 130 ℃, column top temperature of 80 ℃ ~ 170 ℃, tower bottom temperature of 180 to 260 ℃, the total pressure drop packing 0.4Kpa ~ 1.0Kpa, controlling the reflux ratio R between 0.4 and 2.5, the theoretical plate number is 4 to 28.

包括间歇蒸馏步骤C)生成的粗二壬基酚回收二壬基酚步骤。 Including batch distillation step C) recovering the resulting crude dinonylphenol dinonylphenol step.

间歇蒸馏塔进料温度为130℃~170℃,塔顶温度为140℃~180℃,塔釜温度为190~270℃,总填料压力降为0.4Kpa~1.0Kpa,回流比R控制在0.1~1.8之间,理论板数为6~26块。 Batch distillation column feed temperature of 130 ℃ ~ 170 ℃, column top temperature of 140 ℃ ~ 180 ℃, tower bottom temperature is 190 ~ 270 ℃, the total pressure drop packing 0.4Kpa ~ 1.0Kpa, controlling the reflux ratio R 0.1 1.8 the number of theoretical plates having 6 to 26.

蒸馏过程回流比R最优控制在0.8~1.5。 Optimal control in the distillation process reflux ratio of 0.8 to 1.5 R.

蒸馏过程理论塔板数为10~15块。 Number of theoretical plates of the distillation process 10 to 15.

精馏过程回流比R最优控制在0.8~1.5。 Optimal control in the distillation process reflux ratio of 0.8 to 1.5 R.

精馏过程理论塔板数为8~14块。 Number of theoretical plates of distillation processes from 8 to 14.

间歇蒸馏塔回流比R控制在0.8~1.3。 Batch distillation column reflux ratio R is controlled to 0.8 to 1.3.

间歇蒸馏塔理论塔板数为10~16块。 Batch distillation column theoretical plate number of 10 to 16.

本发明的特点是在“蒸发—蒸馏—精馏—间歇蒸馏”四步法工艺中,采用四个塔(或一蒸发器和三塔),前面三个塔(或一蒸发器和两塔)采用连续蒸馏的操作方式,后一个塔采用间歇蒸馏的操作方式,来精制壬基酚,提高其收率,并且回收利用二壬基酚。 Feature of the invention is to "evaporate - Distillation - Distillation - batch distillation" four-step process, using four towers (or three towers and an evaporator), the first three columns (or two columns and an evaporator) using continuous distillation operation, a column after distillation using a batch mode of operation, to refine nonylphenol, improve the yield, the recycling and dinonylphenol. 各塔的作用如下:a.采用连续蒸发工艺,利用蒸发塔(器),在短时间、较低温度下脱除大部分苯酚;控制底部出料含酚量低于5%。 The role of the column as follows: a continuous evaporation process, the use of the evaporator tower (), a short time to remove most of the phenol at low temperatures; the bottom of the discharge control phenol content less than 5%.

b.物料经过连续运转的脱残酚塔,苯酚从塔底脱出,塔釜流出含少量重化物的壬基酚。 B. Material residues after removal of phenol column continuous operation, coming out from the bottom of phenol, nonyl phenol bottoms effluent containing a small amount of heavy compounds.

c.物料经连续壬基酚精馏塔处理,壬基酚从塔顶馏出。 C. fractionator materials are continuously processed nonylphenol, nonylphenol distilled off from the top of the column. 塔底获得重化物,并控制使壬基酚精馏塔顶产品的苯酚含量不大于0.05%。 Heavy bottoms obtained compound, and to control the content of phenol nonylphenol rectification column top product is not more than 0.05%.

d.对壬基酚精馏塔底流出物采用间歇蒸馏的方式,回收重化物中的壬基酚和二壬基酚,增加高附加值产品的总收率。 D. nonylphenol substrate fractionator effluent distillation using a batch mode, was recovered weight of nonylphenol and dinonylphenol, to increase the overall yield of high value-added products.

本工艺的核心是通过合理的设计和组合工艺过程,使苯酚、壬基酚和二壬基酚得以有效的分离。 The core of the process is through rational design and combination process, phenol, nonylphenol and dinonylphenol are effectively separated. 首先通过两段蒸馏工艺有效的脱除苯酚,在一段脱酚工艺中,先使苯酚降低至5%左右,而在二段工艺中,则进一步脱除残余苯酚。 Through two stages of a distillation process effective removal of phenol in the phenol removal period of the process, to reduce the phenol to about 5%, while in the two-stage process, it is further remove residual phenol. 由于有了一段脱酚的工艺。 Thanks phenols off process section. 物料中的苯酚含量得以大幅度降低,这样使得二段脱残酚塔的负荷得以大幅度降低,通过工艺优化可以极大的提高精馏效果。 A phenol content in the material is greatly reduced, so that the load residue removal Sec phenol column can be greatly reduced by the process of optimization can greatly improve the effect of rectification. 通过蒸馏的过程,使苯酚和烷基酚得到彻底的分离。 By a distillation process, phenol and alkylphenol be completely separated. 然后对脱除了苯酚的壬基酚进一步进行精制,以分离其中的二壬基酚。 Then further purified in addition to removal of phenol nonylphenol, dinonylphenol to separate them. 经过上述两个过程后,苯酚、壬基酚和二壬基酚得到彻底的分离。 After the above two processes, phenol, nonylphenol and dinonylphenol be completely separated. 并且粗壬基酚中所含的三种主要组分都得到充分得精制。 Nonylphenol and the crude three main components are fully contained in refining. 其中的苯酚可以继续进行烷基化反应,而二壬基酚也可以得到充分利用。 Wherein the phenol alkylation reaction can proceed, and dinonyl phenol may be fully utilized. 本工艺通过塔的组合来实现上述目标。 This process is used to achieve these goals through the column combination. 其中关键的是脱残酚塔和回收塔。 The key is the removal of residual phenol column and recovery column.

本发明所具有的3具塔,分别用于脱残酚(T-1),壬基酚精馏(T-2)和二壬基酚回收(T-3),前两塔连续运转,二壬基酚回收塔间歇操作。 The present invention has three columns, respectively, for the removal of phenol residues (T-1), nonylphenol distillation (T-2) and the two recovered nonylphenol (T-3), the first two columns of continuous operation, two nonylphenol recovery column intermittent operation. 各塔的操作要点是:T-1塔底流出物的苯酚含量低于0.02%,从而保障最终壬基酚产品的苯酚含量符合要求;T-2顶控制二壬基酚含量<0.70%,允许塔底流出物的壬基酚含量高一些;T-3在二壬基酚产品质量允许的前提下,要尽可能提高拔出率。 Operation points of each column are: T-1 content of phenol bottoms stream is less than 0.02%, in order to protect the final product phenol content of nonylphenol compliance; T-2 dinonyl top control content <0.70%, allowing nonylphenol high content of some bottoms stream; T-3 under the premise of product quality dinonylphenol allowed, as far as possible to improve the extraction rate. 三具塔的底部都设置了氮气气提设施,氮气一方面起着提供分压,降低塔釜温度的作用,另一方面使物料始终有氮气伴随,起隔绝空气、减少氧化的作用。 The bottom of column three are provided with a nitrogen stripping facility, nitrogen plays an aspect to provide a partial pressure lowering effect of the tower bottom temperature, on the other hand the material is always accompanied with a nitrogen, isolated from the air, reduce the effect of oxidation.

其它操作变量如各塔的进料温度、塔顶和塔釜的温度对各反应段的分离要求都有重要的影响,所以建议选择的温度在要求的范围内。 Other operating variables such as feed temperature of each column, the overhead and bottoms temperature of the reaction section are separated have a major impact requirements, it is recommended to select the range of temperature required.

回流比R和精馏塔理论板数N,是通过精馏效果、投资与能耗等之间的协调优化确定的。 R rectification column reflux ratio and the number of theoretical plates N, by optimizing the coordination between the rectification effect, the investment and energy consumption determined. 减小R和增加N,都能够改善精馏效果,当在最小回流比下操作时,所需要的理论塔板层数为无限多。 Increase and decrease R N, rectification effect can be improved, when operating at minimum reflux ratio, the number of layers required for the infinite number of theoretical plates. 因此,实际回流比是介于两种极限情况之间。 Therefore, the actual reflux ratio is between the two limiting cases. 而是通过经济衡算决定,即操作费用和设备折旧费用之和为最低时的回流比,是适宜的回流比。 But it decided to count through economic scale, that is, the sum of the depreciation expense for the reflux ratio at the lowest operating cost and equipment, are suitable reflux ratio. 当R=Rmin时,塔板层数N=∞,故设备费用无限大。 When R = Rmin, trays layers N = ∞, so the equipment cost is infinite. 但R稍大于Rmin后,塔板层数从无限多减少至有限层数,故设备费急剧降低。 But slightly larger than the Rmin of R, the number of layers is reduced from an infinite number of trays to a limited number of layers, so that equipment costs drastically reduced. 当R继续增大时,塔板层数虽然仍可减少,但减少速率变得缓慢。 When R continues to increase, although trays may still reduce the number of layers, but the rate of decrease became slow. 但设备尺寸增加,费用增加,因此理论塔板数和回流比是根据工艺要求协调确定的。 But the apparatus size increases, the cost, and therefore the number of theoretical plates and a reflux ratio are determined according to process requirements coordinated.

在以上条件范围内选择工艺参数和操作变量,通过本工艺的实施,能快速有效的将壬基酚中的酚含量降至很低,解决色泽稳定性问题,同时可以进一步提高壬基酚的收率,回收纯度较高的二壬基酚,提高高附加值产品的收率。 Process parameters and operating variables within the above range of conditions, by the process of the present embodiment can be quickly and effectively reduced the phenols content nonylphenol low solution color stability, and can further improve the yield of nonylphenol rate, a high purity recovery dinonylphenol, to improve the yield of high value-added products.

本发明提供的工艺可以最大限度的回收产品。 The process of the invention can provide maximum product recovery. 只有获得纯度较高的二壬基酚,才可以较好的利用二壬基酚,回收的苯酚可以进一步参与烷基化反应。 Only dinonylphenol obtained with high purity, better use can dinonylphenol recovered phenol may be further involved in the alkylation reaction. 高附加值产品二壬基酚的回收利用有着十分重要的意义。 High value-added products dinonyl recycling has great significance.

附图说明 BRIEF DESCRIPTION

图1波兰壬基酚工艺流程图图2Hüels公司壬基酚工艺流程图图3兰炼壬基酚工艺流程图图4壬基酚苯酚回收及产品精制新工艺流程简图具体实施方式实施例11蒸发:脱苯酚采用薄膜蒸发器来脱除反应物料当中的大部分苯酚,其目的通过高效蒸发器来脱除反应器出来的物料当中的大部分苯酚,以降低其后脱残酚塔的负荷。 FIG. 1 process flow diagram Poland 2Hüels 4 Nonylphenol Nonylphenol phenol recovery and upgrading new process diagram DETAILED DESCRIPTION Example 11 was evaporated Company nonylphenol flow chart in FIG. 3 process flow diagram nonylphenol Lanlian : phenol removal using a thin film evaporator to remove most of the reaction mass among the phenol, used to remove most of the object out of the reactor through which the material phenol efficiency evaporator, to reduce the load of the subsequent removal of residual phenol column. 进料温度控制在70-150℃。 The feed temperature was controlled at 70-150 ℃.

2蒸馏:脱残酚A:脱除了大部分苯酚的混合物料从薄膜蒸发器通过管线连续进入进料中间罐,物料由进料泵输送进入板框过滤机,滤掉其中的树脂碎粒后,在进料预热器加热,使物料的温度升高并达到工艺要求的70℃后,其出口温度由脱残酚塔进料段温度控制来调节。 2 Distillation: off residual phenol A: freed from most of the phenol from the mixed material film evaporator through line continuously fed into the tundish material from the feed is pumped into the frame filter, wherein the resin is filtered off after nibs, after heating the feed preheater, the temperature of the material rises and process requirements of 70 ℃, outlet temperature controlled to adjust the temperature of the feed section of the column by the removal of phenol residues.

B:给脱残酚塔建立液面。 B: A residue removal column phenol established level. 手动打开进料管上的控制阀复线,并将其流量调至最大,使脱残酚塔液面升高。 Manually open the control valve on the bifurcated feed tube, and the flow rate was adjusted to maximum, the stripper column liquid level rises the residual phenol.

C:当脱残酚塔液面升高至50%时,开动塔底出料泵使塔内物料循环;启动真空泵给脱残酚塔建立真空,并调节真空度使塔内残压不大于2.7kPa。 C: When the phenol residue removal column was raised to 50% level, the discharge pump actuated bottoms circulating material in the column; the vacuum pump to create a vacuum tower phenol residue removal, and adjusting the degree of vacuum tower residual pressure not greater than 2.7 kPa.

D:打开进料温度控制阀,将进料流量调至所需值,同时关闭进料温度控制复线阀,使进料流量达到工艺要求的1100kg/h。 D: temperature of the feed control valve is opened, the intake flow rate was adjusted to the desired value of the material, while closing the bifurcated feed temperature control valve, the feed flow rate to process requirements of 1100kg / h.

E:同时打开塔底再沸器的加热复线阀给塔内物料快速升温,当塔底温度达到工艺值的要求的175℃后,打开塔底温度控制阀,同时关闭塔底再沸器的加热复线阀,并根据塔底温度的变化调整控制阀上述设定值。 E: open at a bottom reboiler heated bifurcated valve material to rapid heating tower, when the process values ​​reach the bottom temperature 175 deg.] C requirements, open bottom temperature control valve, while closing a bottom reboiler heated Pipeline valve, the valve and change the setting value adjustment control according to the column bottom temperature.

F:当脱残酚塔顶温度达到工艺要求的45℃温度时,将出料流程改到物料中间罐并通知分析部门分析脱残酚塔抽出物料当中的苯酚含量,当脱残酚塔底抽出物料合格后,将物料抽出流程改到正常罐,保持上述工艺,通过相关控制阀控制进料流量和温度、塔底和塔底温度,保证塔内各点的温度和塔内液面保持在工艺要求的范围之内。 F: When the temperature 45 ℃ phenolic residues removal process requirements overhead temperature of the material to change the material flow and can notify the intermediate sector analysis Analysis phenol content of phenol removal residual material extracted from among the column, bottoms out when the removal of phenol residues after passing the material, the material is changed to the normal flow out the tank, holding the process, the associated control valve controls the feed flow rate and temperature, a bottom and a bottom temperature of the column to ensure that the temperature of each point of the column and the liquid level in the process within the scope of the claims.

脱残酚塔顶馏出的是残留在物料中的苯酚,以及部分低碳烷基酚。 Off overhead phenol residues remaining in the material of phenol, alkylphenols and lower portions. 需要说明的是最终产品中的低碳烷基酚含量取决于进入反应系统的原料壬烯中的低碳数烯烃含量,它们与苯酚反应生成的烷基酚沸点大于苯酚,小于壬基酚,难以依靠蒸馏除去,除非设置专门的分离塔,否则即使把它们从脱残酚塔顶分了出去,还是存在于体系内,会引起积累,造成操作紊乱。 Note that the lower the content of low carbon number olefins alkylphenol content in the final product depends on the feedstock entering the reactor system in nonene, they react with the phenol produced is greater than the boiling point of phenol, alkylphenols, nonylphenol less than difficult rely distilled off, unless special separation column is provided, or even break them off from the top of the column out residual phenol, or present in the system, can cause accumulation, causing operation disturbances. 脱残酚塔顶馏出物冷凝后依靠重力流入反应系统的苯酚进料罐。 After removal gravity residual phenol condensed overhead into the reaction system phenol feed tank. 脱残酚塔在2.7kPa残压下操作,回流比为0.8。 Removal residual phenol column at 2.7kPa residues depressing operation, a reflux ratio of 0.8. 塔底再沸器向脱残酚塔补充热量,与氮气共同作用,进一步降低流出物——粗产物的酚含量。 A bottom reboiler to add heat removal column phenolic residues, cooperates with nitrogen, further reduced effluent - phenol content of the crude product. 塔底流出量由液位控制仪控制,物料依靠重力,进入相壬基酚中间罐。 A bottoms outflow level control device controls the material by gravity, into the intermediate tank with nonylphenol.

3精馏:壬基酚精馏壬基酚精馏塔的进料泵将粗壬基酚从粗壬基酚中间罐抽出,经过换热器加热后,输送到精馏塔。 3 Distillation: Nonylphenol Nonylphenol distillation rectification column The crude feed pump Nonylphenol Nonylphenol tundish from the crude extracts, after the heat exchanger is heated, conveyed to rectification column. 精馏塔蒸发量大,为了缩短物料在塔底的停留时间,采用液混相进料。 Fractionator evaporation, in order to shorten the residence time of the material at the bottom, by liquid-phase feed mixture. 精馏塔同样在2.67kPa残压下操作,塔顶回流及温度控制方式与脱残酚塔相同,回流比为0.8。 Also in the distillation column residues 2.67kPa depressing operation, temperature control and overhead reflux with removal of phenol residues same column, a reflux ratio of 0.8. 塔顶馏出的壬基酚产品,经过换热器,进入壬基酚接受罐,然后输送出装置。 The overhead product of nonylphenol, through the heat exchanger, enters the receiving tank nonylphenol, then conveyed out of the device. 在塔底再沸器和氮气共同作用,从塔底物料中回收壬基酚。 Cooperate further reboiler and nitrogen, the material recovered from the bottom of nonylphenol at the bottom. 塔底流出量由液位控制仪控制,物料依靠重力,进入粗二壬基酚中间罐,也可以经过管线直接进入二壬基酚回收塔。 A bottoms outflow level control device controls the material by gravity, into the crude dinonylphenol tundish, may be entered directly via line dinonylphenol recovery column.

4间歇蒸馏:二壬基酚回收粗二壬基酚经过预热器,进入回收塔。 4 batch distillation: dinonyl recovered crude dinonylphenol through preheater, into the recovery column. 回收塔在1.35kPa残压下间歇操作,塔顶回流及温度控制方式与脱残酚塔相同。 Recovery column pressure at 1.35kPa residues intermittent operation, temperature control and overhead reflux to the column the phenol removal identical residues. 塔顶馏出物是二壬基酚和残留在精馏塔底流出物中的壬基酚,经过冷凝器冷却,进入二壬基酚接受罐,然后输送出装置。 Overhead nonylphenol and di substrate remaining in the distillation column nonylphenol effluent, through the condenser was cooled, enters the receiving tank dinonylphenol, then conveyed out of the device. 塔底重沸器和氮气提高二壬基酚的回收率。 Reboiler dinonylphenol and increase the recovery of nitrogen. 塔底流出的重化物进入重化物中间罐,然后输送出装置。 The bottoms stream of heavy weight compounds from entering a tundish, then the delivery device.

5添加色泽稳定剂壬基酚从管线计量进入色泽稳定剂溶液配制罐,搅拌下加入色泽稳定剂,配制成规定浓度的溶液,两具溶液配制罐轮流使用。 5 nonyl phenol was added into the color and color stability stabilizer solution can be formulated from the metering line, color stabilizers added with stirring to prepare a solution of a predetermined concentration, two solutions were prepared using the pot turns. 溶液用泵计量送入管线,与壬基酚一同通过静态混合器进行混合。 Solution feed line with the metering pump, together with nonylphenol mixed by a static mixer. 实施过程具体的工艺流程见图4。 Specific embodiments of the process of the process shown in Figure 4.

各塔的操作条件见表1:表1各塔操作参数 The operating conditions of each column in Table 1: Table 1 in each column operating parameters

壬基酚苯酚回收精制过程试验中,在改变混合物料的组成,其它操作条件不变的情况下,做多组实验进行检验,具体数据见表2。 Nonylphenol phenol recovery test refining process, in the case of changing the composition of the mixed material, the other operating conditions remain unchanged, multiple set of experiments tested do, particularly the data in Table 2.

表2精制前后各组组成 Table 2 in each group before and after refining Composition

精制前的物料混合按百份比配制,精制后各物质组成是用安捷伦气相色谱仪GC6820分析得出。 Materials prepared by mixing before purification by percentage, each consisting refined analysis was obtained using an Agilent GC6820 gas chromatograph. 从试验的数据中我们可以看到,精制后的产品能够满足壬基酚产品的质量要求,表明在工艺操作条件不变的情况下,在壬基酚生产的产物的组成发生变化时,按照规定的操作条件,进行壬基酚苯酚的回收精制,完全可以达到产品的质量要求。 We can see from the test data, the refined products can meet the quality requirements of the product of nonylphenol, indicate that in the case where the same process conditions, in the composition of the product produced nonylphenol changes, in accordance with operating conditions, recovering purified phenol nonylphenol, can meet the quality requirements of the product.

实施例2各塔的操作条件见表3:表3各塔操作参数 Each column operating conditions of Example 2 shown in Table 3: Table 3 Operating parameters of each column

添加色泽稳定剂后,精制前后组成具体数据见表4。 After the addition of color stabilizers, particularly before and after purification composition data in Table 4.

表4精制前后组成 Table 4 composition before and after refining

壬基酚、苯酚回收精制过后,所获得的壬基酚产品的质量指标达到:壬基酚纯度≥99.00%,二壬基酚≤0.70%,低碳烷基酚含量≤0.25%,苯酚含量≤0.05%,色度≤50铂钴号。 Nonylphenol, phenol recovery after purification, nonylphenol quality indicators obtained product reached: nonylphenol purity ≥99.00%, dinonylphenol ≤0.70%, a low carbon content alkylphenol ≤0.25%, a phenol content ≤ 0.05%, ≤50 platinum-cobalt color number.

精制前的物料混合按百份比配制,精制后各物质组成是用安捷伦气相色谱仪GC6820分析得出。 Materials prepared by mixing before purification by percentage, each consisting refined analysis was obtained using an Agilent GC6820 gas chromatograph. 从试验的数据中可以看到,精制后的产品能够满足壬基酚产品的质量要求,表明在工艺操作条件不变的情况下,在壬基酚生产的产物的组成发生变化时,按照规定的操作条件,进行壬基酚苯酚的回收精制,完全可以达到产品的质量要求。 Can be seen from the test data, the refined products can meet the quality requirements of the product of nonylphenol, it indicates that in the case where the same process conditions, in the composition of the product produced nonylphenol change, according to a predetermined operating conditions, recovering purified phenol nonylphenol, can meet the quality requirements of the product.

Claims (9)

  1. 1.一种壬基酚精制工艺,精制壬烯和苯酚在催化剂的作用下化合而成的工业壬基酚,其特征在于:包括以下过程,a)蒸发:去除工业壬基酚中的大部分苯酚,得到蒸发器底部出料;b)蒸馏:去除蒸发器底部出料中的苯酚,得到粗壬基酚,蒸馏塔进料温度为70℃~120℃,塔顶温度为40℃~85℃,塔釜温度为170~215℃,总填料压力降为0.4Kpa~1.0Kpa,回流比R控制在0.5~2之间,理论塔板数为6~30块;c)精馏:精馏粗壬基酚,得到精制壬基酚和粗二壬基酚,精馏塔进料温度为90℃~130℃,塔顶温度为80℃~170℃,塔釜温度为180~260℃,总填料压力降为0.4Kpa~1.0Kpa,回流比R控制在0.4~2.5之间,理论塔板数为4~28块。 A nonylphenol refining process, refined nonene and phenol compound in the presence of a catalyst obtained by industrial nonylphenol, characterized by: comprising the following process, A) evaporation: the removal of most industrial nonylphenol phenol, to give the bottom of the evaporator feed; b) distillation: removing the bottom of the evaporator feed phenol, nonyl phenol to give a crude distillation column feed temperature of 70 ℃ ~ 120 ℃, column top temperature of 40 ℃ ~ 85 ℃ tower bottom temperature is 170 ~ 215 ℃, the total pressure drop packing 0.4Kpa ~ 1.0Kpa, controlling the reflux ratio R between 0.5 and 2, the theoretical plate number is from 6 to 30; c) distillation: distillation of crude nonylphenol, nonylphenol and purified to give the crude dinonylphenol, fractionator feed temperature of 90 ℃ ~ 130 ℃, column top temperature of 80 ℃ ~ 170 ℃, tower bottom temperature is 180 ~ 260 ℃, total filler pressure drop 0.4Kpa ~ 1.0Kpa, controlling the reflux ratio R between 0.4 and 2.5, the theoretical plate number is 4 to 28.
  2. 2.根据权利要求1所述的一种壬基酚精制工艺,其特征在于:所述工艺还包括间歇蒸馏步骤C)生成的粗二壬基酚回收二壬基酚步骤。 One kind of nonylphenol according to claim 1 of the refining process, characterized in that: said process further comprising a batch distillation step C) recovering the resulting crude dinonylphenol dinonylphenol step.
  3. 3.根据权利要求2所述的一种壬基酚精制工艺,其特征在于:间歇蒸馏塔进料温度为130℃~170℃,塔顶温度为140℃~180℃,塔釜温度为190~270℃,总填料压力降为0.4Kpa~1.0Kpa,回流比R控制在0.1~1.8之间,理论板数为6~26块。 A purification process according nonylphenol according to claim 2, wherein: batch distillation column feed temperature of 130 ℃ ~ 170 ℃, column top temperature of 140 ℃ ~ 180 ℃, tower bottom temperature of 190 to 270 deg.] C, the total pressure drop packing 0.4Kpa ~ 1.0Kpa, reflux ratio R is controlled between 0.1 to 1.8, the theoretical plate number is from 6 to 26.
  4. 4.根据权利要求1所述的一种壬基酚精制工艺,其特征在于:蒸馏过程回流比R最优控制在0.8~1.5。 4. A purification process according to any preceding claim nonylphenol in claim 1, wherein: the distillation process was refluxed for optimal control ratio 0.8 - 1.5 R.
  5. 5.根据权利要求1所述的一种壬基酚精制工艺,其特征在于:蒸馏过程理论塔板数为10~15块。 A purification process according nonylphenol according to claim 1, wherein: theoretical plate number of the distillation process 10 to 15.
  6. 6.根据权利要求1所述的一种壬基酚精制工艺,其特征在于:精馏过程回流比R最优控制在0.8~1.5。 A purification process according nonylphenol according to claim 1, wherein: the distillation process was refluxed for optimal control ratio 0.8 - 1.5 R.
  7. 7.根据权利要求1所述的一种壬基酚精制工艺,其特征在于:精馏过程理论塔板数为8~14块。 A purification process according nonylphenol according to claim 1, wherein: the theoretical plate number of distillation processes from 8 to 14.
  8. 8.根据权利要求3所述的一种壬基酚精制工艺,其特征在于:间歇蒸馏塔回流比R控制在0.8~1.3。 8. A purification process according to any preceding nonylphenol claim 3, wherein: R a batch distillation column reflux ratio of 0.8 to 1.3 in the control.
  9. 9.根据权利要求3所述的一种壬基酚精制工艺,其特征在于:间歇蒸馏塔理论塔板数为10~16块。 A purification process according nonylphenol according to claim 3, characterized in that: a batch distillation column theoretical plate number of 10 to 16.
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CN101913994A (en) * 2010-08-24 2010-12-15 江苏凌飞化工有限公司 Method for producing nonyl phenol
CN103265408A (en) * 2013-05-31 2013-08-28 滁州市润达溶剂有限公司 Refining method of nonyl phenol
CN103265410A (en) * 2013-05-31 2013-08-28 滁州市润达溶剂有限公司 Refining method of nonyl phenol
CN104387239A (en) * 2014-11-25 2015-03-04 江苏凌飞科技股份有限公司 Method for increasing content of para-nonylphenol in nonylphenol product

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Publication number Priority date Publication date Assignee Title
CN101913994A (en) * 2010-08-24 2010-12-15 江苏凌飞化工有限公司 Method for producing nonyl phenol
CN101913994B (en) 2010-08-24 2012-01-11 江苏凌飞科技股份有限公司 Method for producing nonyl phenol
CN103265408A (en) * 2013-05-31 2013-08-28 滁州市润达溶剂有限公司 Refining method of nonyl phenol
CN103265410A (en) * 2013-05-31 2013-08-28 滁州市润达溶剂有限公司 Refining method of nonyl phenol
CN103265410B (en) * 2013-05-31 2015-04-15 滁州市润达溶剂有限公司 Refining method of nonyl phenol
CN103265408B (en) * 2013-05-31 2016-01-20 滁州市润达溶剂有限公司 A method for purifying nonylphenol
CN104387239A (en) * 2014-11-25 2015-03-04 江苏凌飞科技股份有限公司 Method for increasing content of para-nonylphenol in nonylphenol product
CN104387239B (en) * 2014-11-25 2016-03-02 江苏凌飞科技股份有限公司 One kind of nonylphenol product alignment method of improving the content of nonylphenol

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